CN105271880A - Cement grinding aid - Google Patents
Cement grinding aid Download PDFInfo
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- CN105271880A CN105271880A CN201510802875.8A CN201510802875A CN105271880A CN 105271880 A CN105271880 A CN 105271880A CN 201510802875 A CN201510802875 A CN 201510802875A CN 105271880 A CN105271880 A CN 105271880A
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- grinding aid
- triethanolamine
- trolamine
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Abstract
The invention discloses a cement grinding aid which is prepared from, by weight, 5-30 parts of modified triethanolamine, 5-20 parts of molasses, 1-4 parts of lignin derivatives, 3-8 parts of chlorinated hydrocarbon and 60-80 parts of water. The cement grinding aid has the advantages that part of modified triethanolamine and chlorinated hydrocarbon act to form quaternary ammonium salt, and accordingly chloride ions are generated in the cement grinding aid under the condition that chlorine salt is not added; the chloride ions can remarkably enhance early strength and the grinding aid effect of cement. Meanwhile, quaternary ammonium salt is not stable, so that the quaternary ammonium salt formed in the cement after construction is decomposed into triethanolamine and chlorinated hydrocarbon again; chlorinated hydrocarbon is volatile so that chlorinated hydrocarbon can volatilize after the cement is constructed, and the problems that steel ribs in concrete are corroded because of the chloride ions, and the service life and durability of the concrete are affected are avoided.
Description
Technical field
The present invention relates to a kind of admixture, more particularly, it relates to a kind of cement grinding aid.
Background technology
Cement grinding aid is a kind of chemical additive improving cement grinding effect and performance, for in the grinding process of cement material, add a small amount of grinding aid can significantly improve mill efficiency or reduce energy consumption, and significantly improve cement unit-hour output and all technical, and don't the performance of infringement cement self.As a kind of chemical activator, grinding aid can improve concrete scroll and excite aquation power, thus improves cement early strength and later strength.The energy consumption that China's Cement industry is produced accounts for 80% of building materials industry energy consumption, account for 8.7% of national industrial production total energy consumption, the benefit that the application of cement grinding aid brings to the Sustainable development of " energy-saving and emission-reduction " of Cement industry and Cement industry, considerably beyond the value of itself, it has become the indispensable subsidiary material of Cement industry.
Disclose a kind of cement grinding aid in documents CN201210265048.6, the mobility of this cement grinding aid high material in mill, effectively reduce grinding machine and cross grinding phenomenon, improve adhesive attraction and self clustering phenomena that material pulls grinding element, liner plate, compartment.
But, in documents, need the salt using the chloride ion-containing such as sodium-chlor and Repone K to increase the effect of grinding aid, but the existence of chlorion easily causes reinforcement in concrete burn into affect concrete work-ing life and weather resistance.
Summary of the invention
For the deficiency that prior art exists, the object of the present invention is to provide a kind of cement grinding aid.This cement grinding aid does not add the salt of the chloride ion-containing such as sodium-chlor and Repone K, but can reach better grinding aid and reinforced effects.
For achieving the above object, the invention provides following technical scheme:
A kind of cement grinding aid, the raw material that to comprise by following parts by weight be major constituent is prepared from:
Modified triethanolamine 5-30 part
Molasses 5-20 part
Lignin derivative 1-4 part
Hydrochloric ether 3-8 part
Water 60-80 part.
The raw material that to comprise by following parts by weight be major constituent is prepared from:
Modified triethanolamine 5-20 part
Molasses 5-15 part
Lignin derivative 1-4 part
Hydrochloric ether 3-6 part
Water 60-80 part.
Described modified triethanolamine is by sad triethanolamine ester: dilaurate triethanolamine ester=0-1:1-0 forms.
Described molasses select the wherein one in beet sirup, cane molasses, glucose sugar molasses.
Described lignin derivative is preferably sodium lignosulfonate.
Described hydrochloric ether select in methylene dichloride, 1,1-ethylene dichloride, 1,2-ethylene dichloride wherein one or more.
A preparation method for modified triethanolamine, is characterized in that: comprise the steps:
Step one: according to mol ratio, sad: trolamine=1.4-1.6:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 130-140 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=1.9-2.3:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=0-1:1-0 mixes.
A preparation method for cement grinding aid, comprises the steps:
5-30 part modified triethanolamine is first poured in reactor by I, then under whipped state, pours 3-8 part hydrochloric ether into carry out mix and blend, reflux 12h, cools stand-by;
II mixture step I obtained is transferred in stirring tank, adds 5-20 part molasses, 1-4 part lignin derivative, 60-80 part water, to stir after 1h discharging and get final product.
By adopting technique scheme, the present invention has some effect following:
1. partially modified trolamine and hydrochloric ether effect form quaternary ammonium salt, thus in cement grinding aid, produce chlorion when not adding villaumite, and chlorion can accomplish remarkable refinforced cement epistasis energy and grinding-aid effect morning.Simultaneously because quaternary ammonium salt has unstable character, therefore the quaternary ammonium salt formed in cement after construction can be decomposed into trolamine and hydrochloric ether again, and hydrochloric ether has easy volatile, so can realize after cement completes construction, alkyl chloride is volatilized, thus can not there is the problem that chlorion causes reinforcement in concrete burn into impact concrete work-ing life and weather resistance;
2. the quaternary ammonium salt that modified triethanolamine and hydrochloric ether are formed has good antimicrobial property, can the sterilization effect of remarkable refinforced cement;
3. the quaternary ammonium salt that modified triethanolamine and hydrochloric ether are formed significantly can strengthen molasses, lignin derivative and the solubility property of other cement additives in water, so when cement is constructed, molasses, lignin derivative and the dispersity of other cement additives in cement can be increased;
4. modified triethanolamine is Esterification from different by trolamine and carries out composite obtaining, and compared to trolamine, modified triethanolamine has better grinding aid and improves the effect of intensity;
5. lignin derivative can not only significantly be surged the intensity of mud, significantly can reduce the consumption of the water in cement use procedure simultaneously.
Embodiment
Embodiment 1-5 is the preparation embodiment of modified triethanolamine.
Embodiment 1
Step one: according to mol ratio, sad: trolamine=1.4:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 130 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=2.2:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=0:1 mixes.
Embodiment 2
Step one: according to mol ratio, sad: trolamine=1.6:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 135 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=2.1:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=0.5:0.5 mixes.
Embodiment 3
Step one: according to mol ratio, sad: trolamine=1.5:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 140 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=2.3:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=0.2:0.8 mixes.
Embodiment 4
Step one: according to mol ratio, sad: trolamine=1.6:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 140 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=2.0:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=0.7:0.3 mixes.
Embodiment 5
Step one: according to mol ratio, sad: trolamine=1.4:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 138 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=1.9:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=1:0 mixes.
Embodiment 6-11 is the preparation embodiment of cement grinding aid.
Embodiment 6
Prepare according to embodiment 1 20 parts of modified triethanolamines are first poured in reactor by I, then under whipped state, pour 8 parts of methylene dichloride into carry out mix and blend, reflux 12h, cool stand-by;
II mixture step I obtained is transferred in stirring tank, adds 20 parts of beet sirups, 4 parts of sodium lignosulfonates, 80 parts of water, to stir after 1h discharging and get final product.
Embodiment 7
Prepare according to embodiment 2 15 parts of modified triethanolamines are first poured in reactor by I, then under whipped state, pour 4 part of 1,1-ethylene dichloride into carry out mix and blend, reflux 12h, cool stand-by;
II mixture step I obtained is transferred in stirring tank, adds 15 parts of glucose sugar molasses, 1 part of sodium lignosulfonate, 60 parts of water, discharging and get final product after stirring 1h.
Embodiment 8
Prepare according to embodiment 35 parts of modified triethanolamines are first poured in reactor by I, then under whipped state, pour 3 part of 1,2-ethylene dichloride into carry out mix and blend, reflux 12h, cool stand-by;
II mixture step I obtained is transferred in stirring tank, adds 10 parts of cane molasses, 2 parts of sodium lignosulfonates, 70 parts of water, to stir after 1h discharging and get final product.
Embodiment 9
Prepare according to embodiment 4 10 parts of modified triethanolamines are first poured in reactor by I, pour into according to mol ratio under whipped state again, by methylene dichloride: 5 parts of mixing solutionss that 1,1-ethylene dichloride=1:1 mixes carry out mix and blend, reflux 12h, cools stand-by;
II mixture step I obtained is transferred in stirring tank, adds 5 parts of cane molasses, 3 parts of sodium lignosulfonates, 75 parts of water, to stir after 1h discharging and get final product.
Embodiment 10
Prepare according to embodiment 5 30 parts of modified triethanolamines are first poured in reactor by I, pour into according to mol ratio under whipped state again, by methylene dichloride: 1,1-ethylene dichloride: 1,6 parts of mixing solutionss that 2-ethylene dichloride=1:1:1 mixes carry out mix and blend, reflux 12h, cools stand-by;
II mixture step I obtained is transferred in stirring tank, adds 13 parts of beet sirups, 2 parts of sodium lignosulfonates, 65 parts of water, to stir after 1h discharging and get final product.
Comparative example
Select embodiment 4 embodiment as a comparison in documents CN201210265048.6
Each component is taken, glycol ether 3.3%, diethanolamine 3%, di-alcohol monoisopropanolamine 23%, molasses 4%, Repone K 1%, sodium-chlor 7%, polyalcohol amine 25%, water 33.7% by following mass percent.
Under normal temperature, molecules surfactant and water are put into reactor, add molasses, Repone K, sodium-chlor, homogenizing (stirring) 15 minutes, add di-alcohol monoisopropanolamine, homogenizing (stirring) 15 minutes, then add glycol ether, diethanolamine, homogenizing (stirring) is after 30 minutes, discharging barrelling after 200 mesh filter screens filter.
Grinding aid is tested
Be applied to by cement grinding aid D1 prepared by the cement grinding aid S6 to S10 prepared according to embodiment 6 to embodiment 10 and the comparative example of equivalent in the little mill test of cement, the formula of cement raw material is (by mass percentage mixture): cement clinker 58.0%, gypsum 4.0%, Wingdale 23.0%, high silica sand rock 4.0%, manganese slag 1.0% and bottom slag 10.0%.6 groups are divided by cement raw material to be placed in laboratory mill respectively, often organize be labeled as successively contrast sample, sample 6, sample 7 ... sample 10, cement grinding aid D1 and S6 to S10 is added respectively to pressing 0.05% of cement raw material quality in contrast sample and sample 6 to 10, and carry out grinding respectively and become cement, the usage quantity of water in record grinding process, calculates the ratio that water consumption accounts for cement.The cement made is detected by GB175-2007 " ordinary Portland cement ", the check data of the cement of gained is in table 1, again according to the one-way analysis of variance method (horizontal α=0.05 of the significance of difference) of Duncan multiple range tests, use spss17.0 data processing software to carry out significance of difference analysis, analytical results is in table 1.
Table 1
Antibacterial experiment
Step 1: be placed on by intestinal bacteria in LB substratum and cultivate, dispersion concentration is 80cfu ﹒ mL
-1, bacterium liquid is divided into 6 parts, records colibacillary starting point concentration C1.In every part of bacterium liquid, add the cement grinding aid made according to comparative example and embodiment 6-10 of equivalent respectively, after 6h, measure colibacillary concentration C 2, and record concentration decrement according to formulae discovery.
Formula: concentration decrement=(C1-C2)/C1.
Step 2: get pneumobacillus again, Bacillus subtilus repeats colibacillary experiment.
Table 2 concentration decrement
As can be seen from Table 1, compared to comparative example, the present invention has better effect on the characterization data of the grinding-aid effect such as fineness, specific surface area.Meanwhile, the present invention also has effect more better than comparative example in 3d ultimate compression strength and 28d ultimate compression strength, and water consumption generally reduces 5 percentage points (with the weight ratio of cement) than comparative example.The present invention simultaneously is obviously better than comparative example especially on anti-microbial property.Problem simultaneously owing to using the cement of cement grinding aid of the present invention to there is not chloride ion corrosion after having constructed, therefore, it is possible to the duration of service and the working strength that greatly increase cement.
As can be seen from some advantage above, cement grinding aid of the present invention has great market outlook, should be applied.
The above is only the preferred embodiment of the present invention, protection scope of the present invention be not only confined to above-described embodiment, and all technical schemes belonged under thinking of the present invention all belong to protection scope of the present invention.It should be pointed out that for those skilled in the art, some improvements and modifications without departing from the principles of the present invention, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a cement grinding aid, is characterized in that: the raw material that to comprise by following parts by weight be major constituent is prepared from:
Modified triethanolamine 5-30 part
Molasses 5-20 part
Lignin derivative 1-4 part
Hydrochloric ether 3-8 part
Water 60-80 part.
2. cement grinding aid according to claim 1, is characterized in that: the raw material that to comprise by following parts by weight be major constituent is prepared from:
Modified triethanolamine 5-20 part
Molasses 5-15 part
Lignin derivative 1-4 part
Hydrochloric ether 3-6 part
Water 60-80 part.
3. cement grinding aid according to claim 1, is characterized in that: according to weight ratio, and described modified triethanolamine is by sad triethanolamine ester: dilaurate triethanolamine ester=0-1:1-0 forms.
4. cement grinding aid according to claim 1, is characterized in that: described molasses select the wherein one in beet sirup, cane molasses, glucose sugar molasses.
5. cement grinding aid according to claim 1, is characterized in that: described lignin derivative is preferably sodium lignosulfonate.
6. cement grinding aid according to claim 1, is characterized in that: described hydrochloric ether select in methylene dichloride, 1,1-ethylene dichloride, 1,2-ethylene dichloride wherein one or more.
7. a preparation method for modified triethanolamine as claimed in claim 1, is characterized in that: comprise the steps:
Step one: according to mol ratio, sad: trolamine=1.4-1.6:1 mixes, the mixture of sad and trolamine and phenol solution are placed in round-bottomed flask, carry out reducing pressure, reacting by heating, temperature of reaction controls at 130-140 DEG C, reaction 8h, evaporate the water that reaction generates, residue is thick product;
Step 2: after underpressure distillation, gained is thick product, be dissolved in octane-iso, in turn with the NaOH aqueous solution and distilled water wash, to remove unreacted n-caprylic acid, corresponding solvent and trolamine, finally evaporate to obtain final product by solvent octane-iso by Rotary Evaporators;
Step 3: according to lauric acid: the mol ratio ratio of trolamine=1.9-2.3:1 weighs lauric acid and trolamine on electronic balance, elder generation in there-necked flask, add lauric acid and to toluic acid, at the added dropping funnel of there-necked flask, constant speed drips trolamine, drip within half an hour, load onto reflux condensing tube, temperature of reaction controls at 140 DEG C, refluxes 0.5 hour, after slightly cold, change water distilling apparatus into, distillation reaction 11.5h, the water evaporating generation is the thick product of reaction;
Step 4: after distillation, gained is thick product, in turn with the aqueous solution and distilled water wash, then is that solvent obtains dilaurate triethanolamine ester after silicagel column separation and purification with methylene dichloride;
Step 5: the dilaurate triethanolamine ester that sad triethanolamine ester step 2 obtained and step 4 obtain is sad triethanolamine ester according to weight ratio: dilaurate triethanolamine ester=0-1:1-0 mixes.
8. a preparation method for cement grinding aid as claimed in claim 1, is characterized in that: comprise the steps:
5-30 part modified triethanolamine is first poured in reactor by I, then under whipped state, pours 3-8 part hydrochloric ether into carry out mix and blend, reflux 12h, cools stand-by;
II mixture step I obtained is transferred in stirring tank, adds 5-20 part molasses, 1-4 part lignin derivative, 60-80 part water, to stir after 1h discharging and get final product.
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| CN114477845A (en) * | 2022-03-21 | 2022-05-13 | 辛集慕湖混凝土有限公司 | Cement grinding aid and preparation method thereof |
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| CN114477845A (en) * | 2022-03-21 | 2022-05-13 | 辛集慕湖混凝土有限公司 | Cement grinding aid and preparation method thereof |
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