CN1613759A - Preparation for boron modified granular silicon sol - Google Patents
Preparation for boron modified granular silicon sol Download PDFInfo
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- CN1613759A CN1613759A CN200410065673.1A CN200410065673A CN1613759A CN 1613759 A CN1613759 A CN 1613759A CN 200410065673 A CN200410065673 A CN 200410065673A CN 1613759 A CN1613759 A CN 1613759A
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- silicon sol
- granular silicon
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Abstract
A production of boron modified particle silica sol is disclosed. It is carried out by acidizing soluble glass by strong acid cation exchange resin, alkalifying, curing, and ultra-filtering concentrating to obtain high specific superficial area particle silica sol. It can be used in various paper pulp, paper maker and paper application with pH between 4-10.
Description
One, technical field
The invention belongs to the paper grade (stock) chemical assistant preparing technical field in the inorganic chemistry.
Two, background technology
In the paper industry, the zero release of effective use of the shaping of page and the quality of water filtering performance, other chemical assistants, good filler and fiber fines retention and paper waste etc. all need realize with retention aid and filtering aid system efficiently.Existing papermaking retention aid and filtering aid system has many kinds, generally it can be divided into types such as single component, two-pack and microparticle retention and drainage system.
Along with the paper machine develops to high speed, maximization and the neutrality direction of manufacturing paper with pulp, in the production process of paper and cardboard, improve with traditional single component or two-pack retention aid and filtering aid system and to keep and water filtering performance, can not get the result who feels quite pleased.The microparticle retention and drainage system that later 1980s occurs, the general macromolecule cation polymer that adds earlier, as cationic polyacrylamide (CPAM) or cationic starch (CS), it is very big to add specific surface area then, the micropartical of band high-density negative charge is (as wilkinite, colloid silica), this system can produce the throwing out that is very beneficial for retention and improves paper formation.At present, typical microparticle retention and drainage system comprises Compozil system of being made up of colloid silica and cationic starch (CS) (Sweden is according to the exploitation of Kano Bell Co.) and the Hydrocol system of being made up of wilkinite and cationic polyacrylamide (CPAM) (allied colloid exploitation), and the Hydrosil system of forming by aluminium hydroxide and cationic starch etc., wherein, with fastest developing speed with the Compzil micropartical retention system of being formed by colloid silica and cationic starch, use also maximum.Although the current microparticle retention and drainage system of using has remarkable advantages at raising performance of paper stock in retention and drainage aiding and paper formation etc., its cost is obviously higher, has restricted its applying on middle low speed paper machine and low and middle-grade paper kind.
The synthetic of granular silicon sol is to pass through ion exchange treatment, be polymerized with water glass.Water glass output greatly, obtain easily, and is cheap, and therefore, the high effective retention that constitutes with granular silicon sol and cationic polymers helps the filter system, has wide development space.About the technology of preparing of granular silicon sol, United States Patent (USP) 2573734,2574902 and 2631134 discloses the method with storng-acid cation exchange resin acidification water glass.But the silicon sol particle diameter of this method preparation is bigger, does not pass through modification again, can not directly use in paper technology.
Improve storng-acid cation exchange resin acidification sodium silicate process, can obtain the granular silicon sol of high-specific surface area.But the granular silicon sol poor stability of high-specific surface area, in order to improve the stability of silicon sol, specific surface area does not descend and the difficult gel that takes place during storage, just need carry out surface modification to silicon sol.
At present, the granular silicon sol that uses in China's paper industry is all from external import.Because highly confidential to the technology of preparing of the granular silicon sol that uses in the papermaking abroad, domestic research to the paper grade (stock) modified granular silicon sol is very few, up to now, does not still have domestic manufacturer and grasps the high density modified granular silicon sol production technology that is used for papermaking.
Three, summary of the invention
The low-cost preparation method who the purpose of this invention is to provide a kind of paper grade (stock) modified granular silicon sol.
Technical solution of the present invention is:
1. the preparation method of a boron modified granular silicon sol, behind the storng-acid cation exchange resin acidified sodium silicate, alkalization, slaking, ultrafiltration and concentration obtain the high-specific surface area granular silicon sol, it is characterized in that adding boride and carry out modification in preparation process.
2. as the preparation method of 1 described boron modified granular silicon sol, it is characterized in that the adding boride carries out modification after with the storng-acid cation exchange resin acidified sodium silicate.
3. as the preparation method of 1 described boron modified granular silicon sol, it is characterized in that using the storng-acid cation exchange resin acidified sodium silicate, when alkalization, add boride and carry out modification.
4. as the preparation method of 1 described boron modified granular silicon sol, it is characterized in that after using storng-acid cation exchange resin acidified sodium silicate, alkalization, slaking, add boride and carry out modification.
5. as described in 1～4, it is characterized in that the boride that is adopted can be magnesium borate or potassium borate, borsyl, sodium tetraborate, ten hydride of sodium tetraborate, five hydride of sodium tetraborate, boric acid.
6. as the preparation method of 1 described boron modified granular silicon sol, it is characterized in that behind ultrafiltration and concentration, adding alcohols or Sodium hexametaphosphate 99, sodium polyacrylate, carboxymethyl cellulose as stablizer.
Four, embodiment
Embodiment 1, uses the storng-acid cation exchange resin acidified sodium silicate, alkalization, adds the method that boride carries out preparing behind modification, the ultrafiltration and concentration boron modified granular silicon sol after the slaking:
A. be 8% (SiO with concentration
2Weight content) water glass, pump pressure is by the highly acidic cation exchange column, obtains the pH value and be 1.2 acidic silicasol;
B. add the alkalization of 18% 8% water glass, reheat to 40 ℃ is incubated 30 minutes and carries out slaking, is cooled to 16 ℃ (normal temperature);
C. add 1.25ml/g (with SiO
2The weight content meter) the modification of 0.1mol/L magnesium borate;
D. ultrafiltration and concentration to 15%;
E. stir adding stablizer polyvinyl alcohol, consumption is 0.05%.
The boron modified granular silicon sol that obtains, specific surface area 839.68m
2/ g, the about 3.25nm of particle diameter, S-value (S-value representation aggregate forms degree) 28.20%, modification degree 5.0%, pH ≈ 9.28, about 6 months of stationary phase.
Boron modified silicasol and cationic starch are constituted the microparticle retention and drainage system, being used for the precipitated chalk is the bleaching wood pulp papermaking of filler, wherein: bleaching needle-point leaf pulp/bleached hardwood pulp is 60/40, bleaching wood pulp/precipitated chalk is 70/30, the boron modified granular silicon sol consumption is 5kg/t (oven dry stock), the cationic starch consumption is 9kg/t (oven dry stock), and the pH value of paper stock is transferred between 6～7.The retention of the tiny component of paper stock is 89.79%, drainage time 6.44 seconds.With the two-pack retention aid and filtering aid system retention 66.4% that cationic starch 8kg/t (oven dry stock) and cationic polyacrylamide 200g/t (oven dry stock) constitute, drainage time was compared in 7.39 seconds, and the retention performance has improved 35.2%, and filter-aid performance has improved 12.9%.
Embodiment 2, use the storng-acid cation exchange resin acidified sodium silicate, add boride during alkalization and carry out modification, prepare the method for boron modified granular silicon sol behind slaking, the ultrafiltration and concentration:
A. be 5.5% (SiO with concentration
2Weight content) water glass, pump pressure is by the highly acidic cation exchange column, obtains the pH value and be 4.1 acidic silicasol;
B. add the alkalization of 6% 5.5% water glass, add 3.2ml/g simultaneously (with SiO
2The weight content meter) the modification of 1mol/L potassium borate;
C. be heated to 37 ℃, be incubated 30 minutes and carry out slaking;
D. ultrafiltration and concentration to 23%;
E. stir adding stablizer Sodium hexametaphosphate 99, consumption is 0.1%.
The boron modified granular silicon sol that obtains, specific surface area 1052.21m
2/ g, the about 2.59nm of particle diameter, S-value 43.66%, modification degree 23.00%, pH ≈ 9.52, about 8 months of stationary phase.
Boron modified granular silicon sol and cationic starch, cationic polyacrylamide are constituted the microparticle retention and drainage system, being used for the grinding calcium carbonate is the bleaching wood pulp papermaking of filler, wherein: bleaching needle-point leaf pulp/bleached hardwood pulp is 60/40, bleaching wood pulp/grinding calcium carbonate is 70/30, the boron modified granular silicon sol consumption is 5kg/t (oven dry stock), the cationic starch consumption is 9kg/t (oven dry stock), the cationic polyacrylamide consumption is 200g/t (oven dry stock), and the pH value of paper stock is transferred between 7～8.The retention of the tiny component of paper stock is 97.5%, drainage time 4.98 seconds.With the two-pack retention aid and filtering aid system retention 76.4% that cationic starch 8kg/t (oven dry stock) and cationic polyacrylamide 200g/t (oven dry stock) constitute, drainage time was compared in 8.94 seconds, and the retention performance has improved 27.6%, and filter-aid performance has improved 44.3%.
Embodiment 3, use the storng-acid cation exchange resin acidified sodium silicate, after the alkalization, add boride and carry out modification, slaking, and ultrafiltration and concentration prepares the method for boron modified granular silicon sol:
A. be 7% (SiO with concentration
2Weight content) water glass, pump pressure is by the highly acidic cation exchange column, obtains the pH value and be 3.2 acidic silicasol;
B. be heated to 50 ℃, add 0.36ml/g (with SiO
2The weight content meter) NaOH (1mol/L) alkalization;
C. add 2.5ml/g (with SiO
2The weight content meter) the 0.5mol/L borsyl, modification, slaking were carried out in 50 ℃ of insulations in 30 minutes;
D. ultrafiltration and concentration to 16%;
E. stir adding stablizer sodium polyacrylate, consumption is 1%.
The boron modified granular silicon sol that obtains, specific surface area 894.92m
2/ g, the about 3.05nm of particle diameter, S-value 12.80%, modification degree 18.60%, pH ≈ 9.83, about 10 months of stationary phase.
Boron modified granular silicon sol and cationic starch, cationic polyacrylamide are constituted the microparticle retention and drainage system, being used for the precipitated chalk is the crushed news slurry papermaking of deinking of filler, wherein: deinking crushed news slurry/precipitated chalk is 80/20, the boron modified granular silicon sol consumption is 5.5kg/t (oven dry stock), the cationic starch consumption is 9kg/t (oven dry stock), the cationic polyacrylamide consumption is 200g/t (oven dry stock), and the pH value of paper stock is transferred between 9～10.The retention of the tiny component of paper stock is 92.8%, drainage time 7.25 seconds.Two-pack retention aid and filtering aid system retention 58.6% with cationic starch 10kg/t (oven dry stock) and cationic polyacrylamide 200g/t (oven dry stock) formation, drainage time was compared in 11.69 seconds, the retention performance has improved 58.3%, and filter-aid performance has improved 38.0%.
Embodiment 4, use the storng-acid cation exchange resin acidified sodium silicate, and alkalization back adds boride and carries out the method that modification, ultrafiltration and concentration prepare boron modified granular silicon sol:
A. be 5% (SiO with concentration
2Weight content) water glass, pump pressure is by the highly acidic cation exchange column, obtains the pH value and be 2.4 acidic silicasol;
B. add the alkalization of 10% 5% water glass;
C. controlling the liquid temperature is 25 ℃, adds 5.0ml/g (with SiO
2The weight content meter) the modification of 0.04mol/L sodium tetraborate, be incubated 30 minutes;
D. ultrafiltration and concentration to 16%;
E. stir adding stablizer carboxymethyl cellulose (CMC), consumption is 0.01%.
The boron modified granular silicon sol that obtains, specific surface area 837.72m
2/ g, the about 3.26nm of particle diameter, S-value 17.14%, modification degree 12.64%, pH ≈ 9.78, about 12 months of stationary phase.
Boron modified granular silicon sol and cationic starch are constituted the microparticle retention and drainage system, being used for the talcum powder is the wheat straw paper pulp papermaking of filler, wherein: wheat straw paper pulp/talcum powder is 80/20, the boron modified granular silicon sol consumption is 5.5kg/t (oven dry stock), and the cationic starch consumption is 10kg/t (oven dry stock).The retention of the tiny component of paper stock is 89.9%, drainage time 7.38 seconds.With the two-pack retention aid and filtering aid system retention 61.4% that cationic starch 13kg/t (oven dry stock) and cationic polyacrylamide 300g/t (oven dry stock) constitute, drainage time was compared in 9.77 seconds, and the retention performance has improved 46.4%, and filter-aid performance has improved 24.5%.
Among the embodiment 1～4, properties-correcting agent all can use magnesium borate or potassium borate, borsyl, sodium tetraborate, borides such as ten hydride of sodium tetraborate, five hydride of sodium tetraborate, boric acid; Stablizer also all can use other alcohols or Sodium hexametaphosphate 99, sodium polyacrylate, carboxymethyl cellulose etc.
Embodiment 5:
Prepare the method for boron modified granular silicon sol and product performance with embodiment 4.
Boron modified granular silicon sol and cationic starch are constituted the microparticle retention and drainage system, being used for the talcum powder is the bleached chemical thermomechanical pulp papermaking of filler, wherein: bleached chemical thermomechanical paper pulp/talcum powder is 80/20, the boron modified granular silicon sol consumption is 5.5kg/t (oven dry stock), the cationic starch consumption is 10kg/t (oven dry stock), and the pH value of paper stock is transferred between 4～5.The retention of the tiny component of paper stock is 86.0%, drainage time 9.81 seconds.Two-pack retention aid and filtering aid system retention 52.6% with cationic starch 13kg/t (oven dry stock) and cationic polyacrylamide 300g/t (oven dry stock) formation, drainage time was compared in 14.36 seconds, the retention performance has improved 63.4%, and filter-aid performance has improved 31.7%.
The boron modified granular silicon sol of the present invention preparation and is compared from the granular silicon sol of national imports such as Sweden, and performance is suitable, and cost obviously descends, and can apply on the various paper pulp between pH4～10, various paper machine and each paper kind fully.
Claims (6)
1. the preparation method of a boron modified granular silicon sol, behind the storng-acid cation exchange resin acidified sodium silicate, alkalization, slaking, ultrafiltration and concentration obtain the high-specific surface area granular silicon sol, it is characterized in that adding boride and carry out modification in preparation process.
2. the preparation method of boron modified granular silicon sol as claimed in claim 1 is characterized in that adding boride after with the storng-acid cation exchange resin acidified sodium silicate carries out modification.
3. the preparation method of boron modified granular silicon sol as claimed in claim 1 is characterized in that using the storng-acid cation exchange resin acidified sodium silicate, adds boride and carry out modification when alkalization.
4. the preparation method of boron modified granular silicon sol as claimed in claim 1 is characterized in that after using storng-acid cation exchange resin acidified sodium silicate, alkalization, slaking, adds boride and carries out modification.
5. as described in the claim 1～4, it is characterized in that the boride that is adopted is magnesium borate or potassium borate, borsyl, sodium tetraborate, ten hydride of sodium tetraborate, five hydride of sodium tetraborate, boric acid.
6. as the preparation method of the described boron modified granular silicon sol of claim 1～4, add alcohols or Sodium hexametaphosphate 99, sodium polyacrylate, carboxymethyl cellulose in the high-specific surface area granular silicon sol that it is characterized in that behind ultrafiltration and concentration, obtaining.
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|---|---|---|---|
| CN200410065673.1A CN1259238C (en) | 2004-11-12 | 2004-11-12 | Preparation for boron modified granular silicon sol |
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|---|---|---|---|
| CN200410065673.1A CN1259238C (en) | 2004-11-12 | 2004-11-12 | Preparation for boron modified granular silicon sol |
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| CN1259238C CN1259238C (en) | 2006-06-14 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101858043A (en) * | 2010-04-30 | 2010-10-13 | 湖北达雅化工技术发展有限公司 | Preparation method for stable borosilicate sol with high specific surface area |
| CN103966890A (en) * | 2013-02-05 | 2014-08-06 | 金东纸业（江苏）股份有限公司 | Papermaking process |
| CN104540376A (en) * | 2014-12-10 | 2015-04-22 | 鹤山市木森木制品有限公司 | Modified fast-growing wood slurry with electromagnetic shielding effect and preparation method thereof |
| CN112041267A (en) * | 2018-03-02 | 2020-12-04 | 诺力昂化学品国际有限公司 | Charge inversion type silica sol |
| CN112138967A (en) * | 2020-09-15 | 2020-12-29 | 宁波太尔炊具有限公司 | Preparation method of wear-resistant ceramic coating non-stick pan |
| CN116143131A (en) * | 2023-03-02 | 2023-05-23 | 衢州博来纳润电子材料有限公司 | Preparation method of boron modified acidic silica sol with low metal ion content |
-
2004
- 2004-11-12 CN CN200410065673.1A patent/CN1259238C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101858043A (en) * | 2010-04-30 | 2010-10-13 | 湖北达雅化工技术发展有限公司 | Preparation method for stable borosilicate sol with high specific surface area |
| CN101858043B (en) * | 2010-04-30 | 2012-07-04 | 湖北达雅化工技术发展有限公司 | Preparation method for stable borosilicate sol with high specific surface area |
| CN103966890A (en) * | 2013-02-05 | 2014-08-06 | 金东纸业（江苏）股份有限公司 | Papermaking process |
| CN103966890B (en) * | 2013-02-05 | 2017-03-22 | 金东纸业（江苏）股份有限公司 | papermaking process |
| CN104540376A (en) * | 2014-12-10 | 2015-04-22 | 鹤山市木森木制品有限公司 | Modified fast-growing wood slurry with electromagnetic shielding effect and preparation method thereof |
| CN112041267A (en) * | 2018-03-02 | 2020-12-04 | 诺力昂化学品国际有限公司 | Charge inversion type silica sol |
| CN112041267B (en) * | 2018-03-02 | 2024-04-09 | 诺力昂化学品国际有限公司 | Charge-reversal silica sol |
| CN112138967A (en) * | 2020-09-15 | 2020-12-29 | 宁波太尔炊具有限公司 | Preparation method of wear-resistant ceramic coating non-stick pan |
| CN116143131A (en) * | 2023-03-02 | 2023-05-23 | 衢州博来纳润电子材料有限公司 | Preparation method of boron modified acidic silica sol with low metal ion content |
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| Publication number | Publication date |
|---|---|
| CN1259238C (en) | 2006-06-14 |
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