CN102627724B - Paper dry intensifier and preparation method thereof - Google Patents
Paper dry intensifier and preparation method thereof Download PDFInfo
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- CN102627724B CN102627724B CN201210088907.9A CN201210088907A CN102627724B CN 102627724 B CN102627724 B CN 102627724B CN 201210088907 A CN201210088907 A CN 201210088907A CN 102627724 B CN102627724 B CN 102627724B
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Abstract
The invention provides a paper dry intensifier and a preparation method thereof. The preparation method comprises the following steps: in nitrogen atmosphere, reacting water, acrylamide, an anionic monomer, a cationic monomer, a cross-linked monomer, a chain transfer agent, other functional monomers and a photoinitiator under ultraviolet irradiation; adding a pH regulator for regulating the pH value to be 4-6; and adding a radical catcher, and mixing to obtain the paper dry intensifier. The intensifier synthesized by the method has the characteristics of low usage amount and good effect. The intensifier can be used in production of various paper such as case board paper, corrugating base paper, coated paper, cop tube paper, specialty paper and the like, and has the effect of improving the paper dry intensity, which is more remarkable when the recovered waste paper is used as papermaking raw materials. The intensifier can have an excellent paper dry enhancement effect without being added with aluminum sulfate.
Description
Technical field
The present invention relates to the auxiliary agent for papermaking, be specifically related to a kind of Dry Strength Resin and preparation method thereof.
Background technology
Dry Strength Resin is a class important chemical that increases paper strength in paper industry, is generally used for compensation and adds the decline of filler or the caused paper intensity of low-grade fiber (as regenerated fibre).Many water miscible, the superpolymer that can form hydrogen bonded with fiber can become Dry Strength Resin.
In recent years, China's waste paper resource utilization rises year by year, and development potentiality is huge.But the raising of the utilization ratio of waste paper means waste paper and recycles the increase of number of times, can cause declining to a great extent of paper strength index, strengthens paper strength so need to add Dry Strength Resin.Along with constantly rising to paper and Board demand in consumption market, pull the rapid growth of Dry Strength Resin demand.Study of Paper-Strengthening Agent Based has been widely used in the production process of all kinds of paper and cardboard, in order to the dry strength of remarkable increase paper and cardboard, reduces high-quality raw material consumption, reduces production costs; Or raising product specification, the more and more higher specification of quality constantly proposing to meet user.
Conventional Dry Strength Resin has natural polymer if starch and modifier (cationic starch, anionic starch, cross-linking starch etc.) thereof, synthetic polymer are as polyacrylamide, polyvinyl alcohol etc. and other water-soluble natural product type Dry Strength Resin (as guar gum and derivative thereof etc.).In most of the cases, only add such material of massfraction 0.1%～0.75% just can reach effectively dry potent fruit.
The best Dry Strength Resin of effect is polyacrylamide and multipolymer thereof at present, comprises anion-polyacrylamide, cationic-type polyacrylamide and amphiprotic polyacrylamide.Wherein amphiprotic polyacrylamide shows best effect.Polyacrylamide also divides direct linkage type and branched chain type structure.The polyacrylamide that the degree of branching is high has better effect.According to the literature, molecular weight is in the good application performance of having of 500,000 left and right.
Main flow and the trend of synthesized high-performance Dry Strength Resin are the branched chain type amphiphilic polymers of synthetic molecular weight and modest viscosity at present.This Dry Strength Resin can play the dry enhancement of good paper in the situation that not adding Tai-Ace S 150.Normal employing adds the method for linking agent to obtain branched chain type Dry Strength Resin, but often has a common problem, is exactly reaction process control problem, and the viscosity of resulting polymers often there will be excessive or too small problem, controls the improper gelation that also often there will be.
Summary of the invention
The object of this invention is to provide a kind of papermaking dry-strengthening agent and preparation method thereof, the above-mentioned defect existing to overcome prior art.
Method of the present invention, comprises the steps:
In nitrogen atmosphere, by water, acrylamide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent, other functional monomers and photoinitiator, in UV-irradiation, 70～95 ℃ are reacted 1.5～2 hours, add pH adjusting agent to regulate pH to 4～6, finally add free radical scavenger, mix, obtain described papermaking dry-strengthening agent, 25 ℃ of viscosity are 3500～5000mPa*s;
In above processing step, the parts by weight of raw material are:
Described cationic monomer is (methyl) acrylyl oxy-ethyl-trimethyl salmiac, (methyl) dimethylaminoethyl acrylate, (methyl) vinylformic acid lignocaine ethyl ester, diallyldimethylammonium chloride, dimethylamino propyl acrylamide etc. with one or more in tertiary amino monomers or quaternary ammonium salt monomer, adds cationic monomer unit can make Dry Strength Resin and paper-making fibre have better bonding force;
Described anionic monomer is one or more in the monomers such as vinylformic acid, methacrylic acid, methylene-succinic acid, toxilic acid, fumaric acid, maleic anhydride, sodium vinyl sulfonate, vinylbenzenesulfonic acid sodium, sodium allyl sulfonate or methallylsulfonic acid sodium or its esters, add anionic moiety can make Dry Strength Resin have larger use range, and can catch the anionic trash in paper pulp;
Described cross-linkable monomer is that di-vinyl monomers (as methylene-bisacrylamide etc.), trivinyl monomer are (as N, N-diallyl acrylamide etc.) or the activated monomer of other tools (as N, N-DMAA etc.) in one or more, the participation of cross-linkable monomer, can make polymkeric substance produce side chain easily;
Described other functional monomers are one or more in some soft monomers (as Hydroxyethyl acrylate, Propylene glycol monoacrylate), hard monomer (as vinylbenzene, methyl methacrylate) or hydrophobic monomer (as alkyl acrylate, alkyl methacrylate etc.), and other functional monomers are in order to adjust the performance of Dry Strength Resin in some special aspects.Soft monomer can improve the performance of Dry Strength Resin aspect paper folding endurance, and hard monomer can be strengthened Dry Strength Resin in the performance of improving on paper ring crush index, and hydrophobic monomer can improve the dispersiveness of Dry Strength Resin in water;
Described photoinitiator is benzophenone, benzophenone soluble derivative, st-yrax analog derivative, fluorescein or eosin etc.;
Described chain-transfer agent is inorganic chain-transfer agent (as sodium bisulfite, Sodium Pyrosulfite and Sulfothiorine etc.), organic chain transfer agent (as positive Dodecyl Mercaptan, tert-dodecyl mercaptan, Thiovanic acid, mercaptoethanol, other materials, Virahol etc. with sulfydryl) or with one or more in allylic monomer;
Described free radical scavenger is various water-soluble stoppers, and preferably Resorcinol, benzoquinones, iron(ic) chloride, neutralized verdigris etc. maybe can consume the material of free radical, as sodium bisulfite or xitix etc.;
Described pH adjusting agent determines as the case may be, when before system pH regulator higher than 6 time, pH adjusting agent is acids (example hydrochloric acid, sulfuric acid, acetic acid, phosphoric acid etc.); When before system pH regulator lower than 4 time, pH adjusting agent is bases, as NaOH or weight concentration ammoniacal liquor that is 10～15% etc.;
Described ultraviolet source is high voltage mercury lamp, and its wavelength is 100～1000nm, and its power is according to the size adjustment of reaction vessel.
The present invention adopts UV-irradiation photoinitiator initiated polymerization to prepare Dry Strength Resin: take acrylamide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent and other functional monomers as raw material, under the existence of photoinitiator, in nitrogen atmosphere with UV-irradiation initiated polymerization, viscosity stops irradiating ultraviolet light after reaching target zone, finishes polyreaction.Due to light-initiated feature, free radical can produce in a short period of time, also can disappear in a short period of time, therefore the method is compared conventional synthetic method and is had simple to operate, viscosity is easy to control, the advantages such as gelation can be effectively prevented, all moderate Dry Strength Resins of molecular weight, the degree of branching and viscosity can be obtained.
By regulating the ratio of soft or hard monomer, the ratio of zwitterion, and by adding cross-linkable monomer to introduce branched structure, make Dry Strength Resin there is good performance, add the performances such as the ring pressure that can improve into well paper after paper pulp, folding, resistance to broken, anti-tensile, paper internal bond strength.In addition, the branched structure that this Dry Strength Resin has and suitable hydrophilic and hydrophobic matter, make it have less viscosity, has good dispersiveness in water, can dilute easily, easy to use.
There is few, the effective feature of consumption with the synthetic Dry Strength Resin of present method.Can in the production of the multiple paper kinds such as boxboard, Corrugating Base Paper, enamelled paper, cop tube paper, speciality paper, use, play the effect that increases paper dry strength, especially, in the time starching as paper making raw material with reclaimed waste paper, effect is more remarkable.Such Dry Strength Resin can have the dry reinforced effects of outstanding paper in the situation that not adding Tai-Ace S 150.
Embodiment
In embodiment, viscosity all adopts Brookfield DV-II type viscometer determining at 25 ℃.
Embodiment 1
. in reactor, add water 405g, acrylamide 118g, methylene-succinic acid 2g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 16g, methylene-bisacrylamide 0.08g, sodium allyl sulfonate 1g, Propylene glycol monoacrylate 4g, ethyl propenoate 2g and benzophenone 1g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 85 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 1.5 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 4500mPa*s, add liquid caustic soda (32%, weight) 1.5g regulates pH to 4, finally add Resorcinol 0.02g, regulating weight solid content to 20% adds water, be the finished product.
Embodiment 2.
In reactor, add water 400g, acrylamide 100g, methylene-succinic acid 2g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 15g, methylene-bisacrylamide 0.08g, sodium allyl sulfonate 0.8g, Propylene glycol monoacrylate 15g, vinylbenzene 5g and benzophenone 0.5g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 75 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 2 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 5000mPa*s, add liquid caustic soda (32% weight) 1.5g to regulate pH to 6, finally add sodium bisulfite 2g, add water and regulate solid content to 20%, be the finished product.
Embodiment 3
. in reactor, add water 410g, acrylamide 110g, maleic anhydride 2g, (methyl) dimethylaminoethyl acrylate 10g, DMAA 0.9g, sodium allyl sulfonate 0.6g, Rocryl 410 15g, vinylbenzene 5g and benzophenone 0.7g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 75 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 2 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 5000mPa*s, add sulfuric acid (15%, weight) adjusting pH to 5, finally add copper sulfate 0.01g, regulating weight solid content to 20%, be the finished product.
Embodiment 4
. in reactor, add successively water 520g, acrylamide 82g, methylene-succinic acid 1g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 9g, methylene-bisacrylamide 0.03g, sodium allyl sulfonate 0.2g, methyl methacrylate 4g, Propylene glycol monoacrylate 1g, ethyl propenoate 1g and benzophenone 0.5g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 85 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 1.5 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 3500mPa*s, add liquid caustic soda (32%, weight) adjusting pH to 6, finally add para benzoquinone 0.01g, regulating weight solid content to 15% adds water, be the finished product.
Embodiment 5
. in reactor, add successively water 570g, acrylamide 82g, toxilic acid 1g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 10g, DMAA 0.5g, Thiovanic acid 0.005g, vinylbenzene 2g, Propylene glycol monoacrylate 1g, ethyl propenoate 5g and eosin 0.7g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 80 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 1.5 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 3500mPa*s, add liquid caustic soda (32%, weight) adjusting pH to 5, finally add Resorcinol 0.01g, regulating weight solid content to 15% adds water, be the finished product.
Embodiment 6.
In reactor, add successively water 500g, acrylamide 80g, vinylformic acid 2g, dimethyl diallyl ammonium chloride 10g, Vinyl toluene 0.5g, sodium bisulfite 0.8g, Propylene glycol monoacrylate 1g, methyl methacrylate ester 5g and benzoin methyl ether 0.7g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 80 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 1.5 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 4500mPa*s, add liquid caustic soda (32%, weight) adjusting pH to 4, finally add Resorcinol 0.01g, regulating weight solid content to 15% adds water, be the finished product.
Embodiment 7.
In reactor, add water 420g, acrylamide 144g, vinylformic acid 3g, dimethyl diallyl ammonium chloride 17g, DMAA 1g, sodium allyl sulfonate 0.6g, Dodecyl Mercaptan 0.002g Propylene glycol monoacrylate 4g, vinylbenzene 2g and benzoin methyl ether 0.5g stir, reactor is vacuumized to logical nitrogen 2～3 times repeatedly, then maintain logical nitrogen, temperature of reaction kettle is risen to 82 ℃, to reaction system irradiating ultraviolet light, in the basic situation that keeps constant temperature, react 2 hours, start afterwards to carry out viscosity test every sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 4500mPa*s, add liquid caustic soda (32%, weight) adjusting pH to 6, finally add Dichlorodiphenyl Acetate copper 0.01g, regulating weight solid content to 30% adds water, be the finished product.
Comparative example 1.
In reactor, add successively water 550g, acrylamide 81g, vinylformic acid 2g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 9g, methylene-bisacrylamide 0.1g, sodium allyl sulfonate 0.1g to stir, logical nitrogen drives oxygen 60 minutes, be warmed up to 60 ℃, add ammonium persulphate 0.5g (being dissolved in 20g water), temperature of reaction kettle is risen to 82 ℃, react viscosity after 30 minutes and increase sharply, temperature rises rapidly, gelation after several minutes.
Comparative example 2.
In reactor, add successively water 550g, acrylamide 81g, vinylformic acid 2g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 9g, sodium allyl sulfonate 0.2g to stir, logical nitrogen drives oxygen 60 minutes, be warmed up to 60 ℃, add ammonium persulphate 0.5g (being dissolved in 20g water), temperature of reaction kettle is risen to 82 ℃, react and after 1 hour, start sampling and detect viscosity.Viscosity adds stopper stopped reaction after reaching 5000mPa*s.Regulate pH to 4, adding water move to weight solid content is 15%.
Comparative example 3.
In reactor, add successively water 550g, acrylamide 81g, vinylformic acid 2g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride 9g, DMAA 0.8g, sodium allyl sulfonate 0.2g stirs, logical nitrogen drives oxygen 60 minutes, be warmed up to 60 ℃, add ammonium persulphate 0.5g (being dissolved in 20g water), temperature of reaction kettle is risen to 82 ℃, react and after 1 hour, start sampling and detect viscosity.Viscosity adds stopper stopped reaction after reaching 3500mPa*s.Regulate pH to 6, adding water move to weight solid content is 15%.The timed interval of viscosity between 3000mPa*s and 10000mPa*s only has 10 minutes, is relatively difficult to control.
Embodiment 8, application example
. adopt reclaimed waste paper case to pull an oar as raw material, beating degree adds Dry Strength Resin to stir 5 minutes after reaching 35 ° of SR, after being shaped, semi-automatic sheet-former adopts the squeezing of standard page squeezing machine, natural air drying, then detects the indexs such as the tensile strength, ring crush intensity, bursting strength, folding endurance, internal bond strength of paper.Dry Strength Resin add-on is 6 ‰ (dry/oven dry stocks).Table 2 has provided the application data of the prepared Dry Strength Resin of aforesaid method.
Table 2. adds the handsheet intensity index (dry/oven dry stock) of Dry Strength Resin
From above-described embodiment, comparative example and application examples, method therefor of the present invention has simple to operate, and viscosity is easy to control, and can effectively prevent the advantages such as gelation.There is good application performance with the Dry Strength Resin of the method synthesized, compare straight chain type Dry Strength Resin (comparative example 2) and have significant advantage, branched chain type Dry Strength Resin (comparative example 3) effect of comparing by general method synthesized has certain advantage.
The above not does any pro forma restriction to technical scheme of the present invention only as part embodiment of the present invention.Any simple modification, equivalent variations and modification that every technical spirit according to the present invention is done above embodiment, all still belong to technical scheme scope of the present invention.
Claims (2)
1. the preparation method of papermaking dry-strengthening agent, it is characterized in that, comprise the steps: in nitrogen atmosphere, by water, acrylamide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent, other functional monomers and photoinitiator, under UV-irradiation, 70～95 ℃ are reacted 1.5～2 hours, add acid or alkali to regulate pH to 4～6, finally add free radical scavenger, mix, obtain described papermaking dry-strengthening agent;
The parts by weight of raw material are:
Described cationic monomer is one or more in (methyl) dimethylaminoethyl acrylate, (methyl) vinylformic acid lignocaine ethyl ester, diallyldimethylammonium chloride, dimethylamino propyl acrylamide or quaternary ammonium salt monomer;
Described anionic monomer is one or more in vinylformic acid, methacrylic acid, methylene-succinic acid, toxilic acid, fumaric acid, maleic anhydride, sodium vinyl sulfonate, vinylbenzenesulfonic acid sodium, sodium allyl sulfonate or methallylsulfonic acid sodium or its esters;
Described cross-linkable monomer is di-vinyl monomers or trivinyl monomer;
Described other functional monomers are Hydroxyethyl acrylate, Propylene glycol monoacrylate, vinylbenzene, alkyl acrylate or alkyl methacrylate;
Described free radical scavenger is Resorcinol, benzoquinones, iron(ic) chloride, neutralized verdigris, sodium bisulfite or xitix;
Described ultraviolet source is high voltage mercury lamp, and its wavelength is 100～1000nm, and its power is according to the size adjustment of reaction vessel.
2. method according to claim 1, is characterized in that, described photoinitiator is benzophenone, benzophenone soluble derivative, st-yrax analog derivative, fluorescein or eosin;
Described chain-transfer agent is sodium bisulfite, Sodium Pyrosulfite, Sulfothiorine, positive Dodecyl Mercaptan, tert-dodecyl mercaptan, Thiovanic acid, mercaptoethanol, other materials with sulfydryl, Virahol or with one or more in allylic monomer;
Described pH adjusting agent determines as the case may be, when before system pH regulator higher than 6 time, pH adjusting agent is that hydrochloric acid, sulfuric acid, acetic acid, phosphoric acid, NaOH or weight concentration are 10～15% ammoniacal liquor.
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| CN102733226A (en) * | 2012-07-16 | 2012-10-17 | 上海殷泰纸业有限公司 | Method for preparing stainless steel interleaving paper by wastepaper |
| CN103408700A (en) * | 2013-07-09 | 2013-11-27 | 上海东升新材料有限公司 | Preparation method of amphoteric dry strength agent |
| CN103772603B (en) * | 2013-11-28 | 2016-01-20 | 杭州杭化哈利玛化工有限公司 | The preparation method of high molecular narrow ditribution crosslinked polyacrylamide and application thereof |
| JP6060314B2 (en) * | 2014-12-08 | 2017-01-11 | ハリマ化成株式会社 | Paper strength enhancer and paper |
| CN105754042A (en) * | 2016-02-19 | 2016-07-13 | 山东源根化学技术研发有限公司 | Polymer for improving internal bond strength of paper and preparation method thereof |
| CN107189008A (en) * | 2017-06-16 | 2017-09-22 | 江苏富淼科技股份有限公司 | A kind of lower molecular weight amphiprotic polyacrylamide and preparation method thereof |
| CN109180861B (en) * | 2018-08-21 | 2021-04-06 | 上海昶法新材料有限公司 | Novel dry strength agent and preparation method thereof |
| CN110029526B (en) * | 2019-03-15 | 2021-09-24 | 中国科学院宁波材料技术与工程研究所 | Paper dry strength agent, preparation method and application thereof |
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| KR100976822B1 (en) * | 2007-09-20 | 2010-08-20 | 주식회사 화성산업 | Dry strength agent of cation block type and producing method thereof |
| CN102121207B (en) * | 2010-12-03 | 2012-09-26 | 江门市高力依科技实业有限公司 | Papermaking dry-strengthening agent |
| CN102115998B (en) * | 2010-12-31 | 2014-01-15 | 永港伟方（北京）科技股份有限公司 | Dry strengthening agent used for making papers and preparation method and application thereof |
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