CN103554345A - Preparation method for negative ion organosilicon modified polyacrylate paper reinforcing agent - Google Patents
Preparation method for negative ion organosilicon modified polyacrylate paper reinforcing agent Download PDFInfo
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- CN103554345A CN103554345A CN201310471311.1A CN201310471311A CN103554345A CN 103554345 A CN103554345 A CN 103554345A CN 201310471311 A CN201310471311 A CN 201310471311A CN 103554345 A CN103554345 A CN 103554345A
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Abstract
The invention relates to a preparation method for a negative ion organosilicon modified polyacrylate paper reinforcing agent. A transparent negative ion organosilicon modified polyacrylate emulsion is obtained by solution polymerization, by using methylacrylic acid, functional vinyl monomers, lipophilic monomers and gamma-methacryloxy propyl trimethoxyl silane as comonomers and isopropanol as a solvent and a chain transfer agent to carry out free radical polymerization of acrylic monomers, and through the steps of cooling, triethylamine neutralization and water dispersion. The obtained negative ion organosilicon modified polyacrylate paper reinforcing agent can not only effectively increase paper surface strength and folding endurance but also increase waterproof property of the paper surface. Besides, due to the addition of gamma-methacryloxy propyl trimethoxyl silane, adhesion properties between fibers and inorganic fillers are increased; and defects of ash and fiber falling during a printing process of the paper. Meanwhile, the product is simple in preparation process, low in raw material cost and simple in glue-applying process and can be easily applied and popularized in real industries.
Description
Technical field
The invention belongs to fine chemicals preparation field, particularly a kind of preparation method of anion organosilicon modified polyacrylate paper strengthening agent.
Background technology
Since the high speed development, the particularly realization of high speed printing technology of modern paper manufacture and printing technology, also more and more higher for paper strength requirement, so increase paper physical intensity, reducing hair and powder dropping in printing process is the basic demand of modern paper industry.The method strengthening for paper physical property at present mainly be take internal sizing agent and Surface Size as main, and paper surface sizing agent is that a class is being covered with paint, lacquer, colour wash, etc. in paperboard surface, improves the chemical assistant of paper physical intensity.The paper surface-sizing agent that China is used mainly contains starch and treated starch, polyvinyl alcohol (PVA), carboxymethyl cellulose (CMC) and water polyacrylic acid emulsion (WPA) etc.Yet after existing paper surface-sizing agent handling of paper, paper folding and wet strength are not fine, and in paper printing, dry linting phenomenon is not improved fully.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of anion organosilicon modified polyacrylate paper strengthening agent, the monomeric species of the method is selected and compositing range changes extensively, preparation process is simple, the paper strengthening agent obtaining not only has the effect that improves paper folding strength, wet tenacity, and there is increase surface strength of paper, reduce the effect of paper hair and powder dropping phenomenon in printing process.
In order to achieve the above object, the technical solution used in the present invention comprises the following steps:
1) press mass fraction, take respectively the acrylic compounds of 1-4 part, the lipophilicity monomer of the functional vinyl monomer of 5-10 part, 20-40 part, the Virahol of the γ-methacryloxypropyl trimethoxy silane of 1-3 part, 10-20 part, the triethylamine of the oil-soluble initiator of 0.5-1 part, 1.5-4 part and the deionized water of 125-150 part; Wherein, described acrylic compounds is acrylic or methacrylic acid;
2) to reactor, add acrylic compounds, functional vinyl monomer, lipophilicity monomer, γ-methacryloxypropyl trimethoxy silicon, Virahol and oil-soluble initiator, then under nitrogen protection in 70-90 ℃ reaction 4-6 hour, obtain system A;
3) system A is cooled to 20-40 ℃, then adds triethylamine, neutralization reaction 20-40 minute, then under agitation adds the deionized water that is heated to 75-95 ℃, then continues to stir to make to be uniformly dispersed, then 70-90 ℃ of insulation 2 hours, obtains system B; Remove the Virahol in system B, the massfraction of Virahol is controlled at below 0.5%, make anion organosilicon modified polyacrylate paper strengthening agent.
Described functional vinyl monomer adopts Hydroxyethyl acrylate, hydroxyethyl methylacrylate, Propylene glycol monoacrylate or Rocryl 410.
Described lipophilicity monomer adopts the mixture of one or both arbitrary proportions in acrylate monomer, methacrylate monomer.
Described acrylate monomer is the mixture of two or more arbitrary proportion in methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate; Methacrylic acid monomer is the mixture of two or more arbitrary proportion in methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, butyl methacrylate.
Described oil-soluble initiator is Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide.
In described step 3), temperature is that the deionized water of 75-95 ℃ is to add under the rotating speed of 1000 revs/min.
It is that the deionized water of 75-95 ℃ adds fashionable stirring velocity that stirring velocity while continue stirring in described step 3) is greater than temperature.
Virahol in described step 3) in system B is to adopt the mode of underpressure distillation to remove.
The present invention adopts silicone-modified polyacrylate, has prepared anion organosilicon modified polyacrylate paper strengthening agent (Si-WPA), and this paper strengthening agent compared with prior art has following beneficial effect:
1) the present invention has added γ-methacryloxypropyl trimethoxy silicon in the process of preparing anion organosilicon modified polyacrylate paper strengthening agent, γ-methacryloxypropyl trimethoxy silicon add the degree of crosslinking that can effectively improve polyacrylic acid ester molecule, strengthen paper fibre bonding force, meanwhile, can also improve paper folding and wet tenacity; In addition, γ-methacryloxypropyl trimethoxy silicon add the adhesiveproperties that can improve organic fibre and mineral filler, reduce the generation of dry linting in paper printing.
2) the anion organosilicon modified polyacrylate paper strengthening agent making through the present invention carries out applying glue to paper, and after applying glue, water polyacrylic acid emulsion can form one deck macromolecular coating at paper surface, can imitate raising surface strength of paper.
3) particle diameter of the anion organosilicon modified polyacrylate paper strengthening agent that the present invention makes is nano level, and therefore, sizability is good, is easily adsorbed onto in paper fibre, improves paper sizing degree, strengthens paper strength.
4) the present invention adopt radical polymerization, by the organosilane-modified anion organosilicon modified polyacrylate paper strengthening agent of preparing, the feature such as the monomeric species of this method is selected and compositing range changes extensively, preparation process is simple; In actual industrial, be easy to application and promote.
In addition, the deionized water of the 75-95 that the present invention adds in step 3) ℃, the deionized water under this temperature range can improve the migration velocity of polymer segment, is conducive to polymkeric substance and disperses in water, obtains clear aqueous polyacrylate dispersion.
Embodiment
Embodiment 1:
1) press mass fraction, take respectively the vinylformic acid of 1 part, the hydroxyethyl methylacrylate of 5 parts, the butyl acrylate of 15 parts, the methyl methacrylate of 5 parts, the γ-methacryloxypropyl trimethoxy silane of 1 part, the Virahol of 10 parts, the Diisopropyl azodicarboxylate of 0.5 part, the triethylamine of 1.5 parts and the deionized water of 125 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add vinylformic acid, hydroxyethyl methylacrylate, butyl acrylate, methyl methacrylate, γ-methacryloxypropyl trimethoxy silane, Virahol and Diisopropyl azodicarboxylate, then pass into nitrogen temperature is risen to 70 ℃, under nitrogen protection, in 70 ℃ of reactions 4 hours, obtain system A;
3) system A is cooled to 25 ℃, then adds triethylamine, neutralization reaction 30 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 80 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 70 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
Embodiment 2:
1) press mass fraction, take respectively the vinylformic acid of 2 parts, the Propylene glycol monoacrylate of 7 parts, the propyl acrylate of 15 parts, the butyl methacrylate of 10 parts, the γ-methacryloxypropyl trimethoxy silane of 1 part, the Virahol of 12 parts, the 2,2'-Azobis(2,4-dimethylvaleronitrile) of 0.7 part, the triethylamine of 2.2 parts and the deionized water of 130 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add vinylformic acid, Propylene glycol monoacrylate, propyl acrylate, butyl methacrylate, γ-methacryloxypropyl trimethoxy silane, Virahol and 2,2'-Azobis(2,4-dimethylvaleronitrile), then after passing into nitrogen, temperature is risen to 75 ℃, under nitrogen protection, in 75 ℃ of reactions 5 hours, obtain system A;
3) system A is cooled to 30 ℃, then adds triethylamine, neutralization reaction 30 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 80 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 75 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
Embodiment 3:
1) press mass fraction, take respectively the vinylformic acid of 3 parts, the Rocryl 410 of 10 parts, the butyl acrylate of 20 parts, the propyl methacrylate of 10 parts, the γ-methacryloxypropyl trimethoxy silane of 2 parts, the Virahol of 15 parts, the dibenzoyl peroxide of 0.7 part, the triethylamine of 2.5 parts and the deionized water of 135 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add vinylformic acid, Rocryl 410, butyl acrylate, propyl methacrylate, γ-methacryloxypropyl trimethoxy silane, Virahol and dibenzoyl peroxide, then after passing into nitrogen, temperature is risen to 85 ℃, under nitrogen protection, in 85 ℃ of reactions 5 hours, obtain system A;
3) system A is cooled to 35 ℃, then adds triethylamine, neutralization reaction 30 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 80 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 85 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
Embodiment 4:
1) press mass fraction, take respectively the vinylformic acid of 4 parts, the Hydroxyethyl acrylate of 10 parts, the ethyl propenoate of 25 parts, the methyl methacrylate of 15 parts, the γ-methacryloxypropyl trimethoxy silane of 3 parts, the Virahol of 20 parts, the Diisopropyl azodicarboxylate of 1 part, the triethylamine of 4 parts and the deionized water of 150 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add vinylformic acid, Hydroxyethyl acrylate, ethyl propenoate, methyl methacrylate, γ-methacryloxypropyl trimethoxy silane, Virahol and Diisopropyl azodicarboxylate, then after passing into nitrogen, temperature is risen to 90 ℃, under nitrogen protection, in 90 ℃ of reactions 6 hours, obtain system A;
3) system A is cooled to 40 ℃, then adds triethylamine, neutralization reaction 30 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 80 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 90 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
Embodiment 5:
1) press mass fraction, take respectively the vinylformic acid of 2.5 parts, the Propylene glycol monoacrylate of 8 parts, the butyl acrylate of 25 parts, the β-dimethyl-aminoethylmethacrylate of 10 parts, the γ-methacryloxypropyl trimethoxy silane of 2 parts, the Virahol of 20 parts, the 2,2'-Azobis(2,4-dimethylvaleronitrile) of 1 part, the triethylamine of 3 parts and the deionized water of 140 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add vinylformic acid, Propylene glycol monoacrylate, butyl acrylate, β-dimethyl-aminoethylmethacrylate, γ-methacryloxypropyl trimethoxy silicon, Virahol and 2,2'-Azobis(2,4-dimethylvaleronitrile), then after passing into nitrogen, temperature is risen to 80 ℃, under nitrogen protection, in 80 ℃ of reactions 6 hours, obtain system A;
3) system A is cooled to 35 ℃, then adds triethylamine, neutralization reaction 30 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 80 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 75 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
It is as shown in table 1 that the paper of the prepared anion organosilicon modified polyacrylate of above-described embodiment 1-5 paper strengthening agent strengthens result:
The anion organosilicon modified polyacrylate paper strengthening agent paper reinforced effects that table 1 the present invention makes
As can be seen from Table 1, the anion organosilicon modified polyacrylate paper strengthening agent that the present invention makes can be imitated and be improved surface strength of paper, paper folding and wet tenacity.
Embodiment 6:
1) press mass fraction, take respectively the methacrylic acid of 2.5 parts, the Propylene glycol monoacrylate of 8 parts, the methyl acrylate of 25 parts, the β-dimethyl-aminoethylmethacrylate of 10 parts, the γ-methacryloxypropyl trimethoxy silane of 2 parts, the Virahol of 20 parts, the 2,2'-Azobis(2,4-dimethylvaleronitrile) of 1 part, the triethylamine of 3 parts and the deionized water of 140 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add methacrylic acid, Propylene glycol monoacrylate, methyl acrylate, β-dimethyl-aminoethylmethacrylate, γ-methacryloxypropyl trimethoxy silicon, Virahol and 2,2'-Azobis(2,4-dimethylvaleronitrile), then after passing into nitrogen, temperature is risen to 80 ℃, under nitrogen protection, in 80 ℃ of reactions 6 hours, obtain system A;
3) system A is cooled to 40 ℃, then adds triethylamine, neutralization reaction 20 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 75 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 80 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
Embodiment 7:
1) press mass fraction, take respectively the methacrylic acid of 3 parts, the Rocryl 410 of 10 parts, the butyl methacrylate of 20 parts, the propyl methacrylate of 10 parts, the γ-methacryloxypropyl trimethoxy silane of 2 parts, the Virahol of 15 parts, the dibenzoyl peroxide of 0.7 part, the triethylamine of 2.5 parts and the deionized water of 135 parts;
2) in the dry flask of the four-hole that reflux condensing tube, airway, thermometer are housed, add methacrylic acid, Rocryl 410, butyl methacrylate, propyl methacrylate, γ-methacryloxypropyl trimethoxy silane, Virahol and dibenzoyl peroxide, then after passing into nitrogen, temperature is risen to 85 ℃, under nitrogen protection, in 85 ℃ of reactions 5 hours, obtain system A;
3) system A is cooled to 20 ℃, then adds triethylamine, neutralization reaction 40 minutes, then under the rotating speed of 1000 revs/min, stir and add the deionized water that is heated to 95 ℃, then improve stirring velocity, high-speed stirring disperses to make for 0.5 hour evenly, 90 ℃ of insulations 2 hours, obtain system B again; The Virahol in system B is removed in underpressure distillation, makes the massfraction of Virahol below 0.5%, makes the yellow blueing light of outward appearance emulsion, is anion organosilicon modified polyacrylate paper strengthening agent.
The present invention adopts solution polymerization process, take methacrylic acid, functional vinyl monomer, lipophilicity monomer, γ-methacryloxypropyl trimethoxy silane is comonomer, the Virahol of usining carries out the radical polymerization of Acrylic Acid Monomer as solvent and chain-transfer agent, through cooling, neutralization, water-dispersion, obtain transparent anion organosilicon modified polyacrylate water miscible liquid.The anion organosilicon modified polyacrylate paper strengthening agent making due to the present invention is through the modification of γ-methacryloxypropyl trimethoxy silane, after applying glue, can improve the bonding force between paper natural organic fiber and mineral filler, from root, improve dry linting phenomenon paper printing process; This type of polyacrylate dispersion is because it can be by regulating the soft or hard monomer ratio regulation and control mechanical strength of filming, so applicable to the top sizing of different deflection paper; By regulatory function monomer consumption, the hydrogen bonded power between adjustable acrylate polymeric and paper fibre, improves paper strength.
Claims (8)
1. a preparation method for anion organosilicon modified polyacrylate paper strengthening agent, is characterized in that, comprises the following steps:
1) press mass fraction, take respectively the acrylic compounds of 1-4 part, the lipophilicity monomer of the functional vinyl monomer of 5-10 part, 20-40 part, the Virahol of the γ-methacryloxypropyl trimethoxy silane of 1-3 part, 10-20 part, the triethylamine of the oil-soluble initiator of 0.5-1 part, 1.5-4 part and the deionized water of 125-150 part; Wherein, described acrylic compounds is acrylic or methacrylic acid;
2) to reactor, add acrylic compounds, functional vinyl monomer, lipophilicity monomer, γ-methacryloxypropyl trimethoxy silicon, Virahol and oil-soluble initiator, then under nitrogen protection in 70-90 ℃ reaction 4-6 hour, obtain system A;
3) system A is cooled to 20-40 ℃, then adds triethylamine, neutralization reaction 20-40 minute, then under agitation adds the deionized water that is heated to 75-95 ℃, then continues to stir to make to be uniformly dispersed, then 70-90 ℃ of insulation 2 hours, obtains system B; Remove the Virahol in system B, the massfraction of Virahol is controlled at below 0.5%, make anion organosilicon modified polyacrylate paper strengthening agent.
2. the preparation method of anion organosilicon modified polyacrylate paper strengthening agent according to claim 1, is characterized in that: described functional vinyl monomer adopts Hydroxyethyl acrylate, hydroxyethyl methylacrylate, Propylene glycol monoacrylate or Rocryl 410.
3. the preparation method of anion organosilicon modified polyacrylate paper strengthening agent according to claim 1, is characterized in that: described lipophilicity monomer adopts the mixture of one or both arbitrary proportions in acrylate monomer, methacrylate monomer.
4. the preparation method of anion organosilicon modified polyacrylate paper strengthening agent according to claim 3, is characterized in that: described acrylate monomer is the mixture of two or more arbitrary proportion in methyl acrylate, ethyl propenoate, propyl acrylate, butyl acrylate; Methacrylic acid monomer is the mixture of two or more arbitrary proportion in methyl methacrylate, β-dimethyl-aminoethylmethacrylate, propyl methacrylate, butyl methacrylate.
5. the preparation method of anion organosilicon modified polyacrylate paper strengthening agent according to claim 1, is characterized in that: described oil-soluble initiator is Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile) or dibenzoyl peroxide.
6. the preparation method of anion organosilicon modified polyacrylate paper strengthening agent according to claim 1, is characterized in that: in described step 3), temperature is that the deionized water of 75-95 ℃ is to add under the rotating speed of 1000 revs/min.
7. according to the preparation method of the anion organosilicon modified polyacrylate paper strengthening agent described in claim 1 or 6, it is characterized in that: it is that the deionized water of 75-95 ℃ adds fashionable stirring velocity that the stirring velocity while continue stirring in described step 3) is greater than temperature.
8. the preparation method of anion organosilicon modified polyacrylate paper strengthening agent according to claim 1, is characterized in that: the Virahol in described step 3) in system B is to adopt the mode of underpressure distillation to remove.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108192025A (en) * | 2018-01-18 | 2018-06-22 | 九洲生物技术（苏州）有限公司 | The preparation method of biological latex modifying agent |
| CN108517716A (en) * | 2018-04-11 | 2018-09-11 | 区文锐 | It is a kind of colored to bake paper and its manufacture craft |
| CN114108371A (en) * | 2021-12-09 | 2022-03-01 | 山东瑞博龙化工科技股份有限公司 | UV-cured paper surface sizing agent and preparation and application thereof |
| CN114133479A (en) * | 2021-12-28 | 2022-03-04 | 张家港凯宝来环保科技有限公司 | Preparation method of high-molecular polymer for thermal transfer printing ink |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108192025A (en) * | 2018-01-18 | 2018-06-22 | 九洲生物技术（苏州）有限公司 | The preparation method of biological latex modifying agent |
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| CN114108371A (en) * | 2021-12-09 | 2022-03-01 | 山东瑞博龙化工科技股份有限公司 | UV-cured paper surface sizing agent and preparation and application thereof |
| CN114133479A (en) * | 2021-12-28 | 2022-03-04 | 张家港凯宝来环保科技有限公司 | Preparation method of high-molecular polymer for thermal transfer printing ink |
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