CN102627724A - Paper dry intensifier and preparation method thereof - Google Patents
Paper dry intensifier and preparation method thereof Download PDFInfo
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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 be used for the auxiliary agent of papermaking, be specifically related to a kind of Dry Strength Resin and preparation method thereof.
Background technology
Dry Strength Resin is the one type of important chemical that increases paper strength in the paper industry, is generally used for the decline that filler or the caused paper intensity of low-grade fiber (like regenerated fibre) are added in compensation.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 the paper and Board demand in the consumption market, spurred the rapid growth of Dry Strength Resin demand.The paper Dry Strength Resin 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; Perhaps improve product specification, to satisfy the increasingly high specification of quality that the user constantly proposes.
Dry Strength Resin commonly used has natural polymer such as starch and modifier (cationic starch, anionic starch, cross-linking starch etc.), synthetic polymer such as SEPIGEL 305, Z 150PH etc. and other water-soluble natural product type Dry Strength Resin (like guar gum and verivate thereof etc.).In most of the cases, such material that only adds massfraction 0.1%~0.75% just can reach effectively does strong effect.
The best Dry Strength Resin of effect is SEPIGEL 305 and multipolymer thereof at present, comprises anion-polyacrylamide, cationic-type polyacrylamide and amphiprotic polyacrylamide.Wherein amphiprotic polyacrylamide shows best effect.SEPIGEL 305 also divides direct linkage type and branched chain type in view of structure.The SEPIGEL 305 that the degree of branching is high has the better application effect.According to bibliographical information, molecular weight is in and has a good applicability ability about 500,000.
The main flow of present synthesized high-performance Dry Strength Resin and the branched chain type amphiphilic polymers that trend is synthetic molecular weight and modest viscosity.This Dry Strength Resin can play good paper and do enhancement under the situation of not adding Tai-Ace S 150.The normal method that adds linking agent that adopts obtains the branched chain type Dry Strength Resin, but often has a common problem, is exactly reaction process control problem, and excessive or too small problem appears in the viscosity regular meeting of resulting polymers, controls improper also regular meeting and gelation occurs.
Summary of the invention
The purpose of this invention is to provide a kind of papermaking Dry Strength Resin and preparation method thereof, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
In nitrogen atmosphere, with water, acrylic amide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent, other functional monomers and photoinitiator, at UV-irradiation; 70~95 ℃ were reacted 1.5~2 hours; Add the pH regulator agent and regulate pH to 4~6, add free radical scavenger at last, mix; Obtain described papermaking Dry Strength Resin, 25 ℃ of viscosity are 3500~5000mPa*s;
In the above process step, raw materials in part by weight is:
Said cationic monomer is that (methyl) acrylyl oxy-ethyl-trimethyl salmiac, (methyl) dimethylaminoethyl acrylate, (methyl) vinylformic acid lignocaine ethyl ester, diallyldimethylammonium chloride, dimethylamino propyl acrylamide etc. are with one or more in uncle's amino monomers or the quaternary ammonium salt monomer, adds cationic monomer unit and can make Dry Strength Resin and paper-making fibre have better bonding force;
Said anionic monomer is one or more in monomers such as vinylformic acid, methylacrylic 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 and can make Dry Strength Resin that bigger use range is arranged, and can catch the anionic trash in the paper pulp;
Said cross-linkable monomer is that di-vinyl monomers (like methylene-bisacrylamide etc.), trivinyl monomer are (like N; N-diallyl acrylic amide etc.) or other have active monomer (like N; N-DMAA etc.) one or more in; The participation of cross-linkable monomer can make polymkeric substance produce side chain at an easy rate;
Said other functional monomers are one or more in some soft monomers (like Hydroxyethyl acrylate, Propylene glycol monoacrylate), hard monomer (like vinylbenzene, TEB 3K) or the hydrophobic monomer (like 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 the paper folding endurance, and hard monomer can be strengthened Dry Strength Resin in the performance of improving on the paper ring crush index, and hydrophobic monomer can improve the dispersiveness of Dry Strength Resin in water;
Said photoinitiator is UVNUL MS-40, UVNUL MS-40 soluble derivative, st-yrax analog derivative, resorcinolphthalein or eosin etc.;
Said chain-transfer agent is inorganic chain-transfer agent (like sodium sulfite anhy 96, Sodium Pyrosulfite and Sulfothiorine etc.), organic chain transfer agent (like other materials of positive Dodecyl Mercaptan, tert-dodecyl mercaptan, Thiovanic acid, mercaptoethanol, band sulfydryl, Virahol etc.) or has in the allylic monomer one or more;
Said free radical scavenger is various water-soluble stoppers, and preferably Resorcinol, benzoquinones, iron(ic)chloride, neutralized verdigris etc. maybe can consume the material of radical, like sodium sulfite anhy 96 or xitix etc.;
Said pH regulator agent confirms that as the case may be when being higher than 6 before the system pH regulator, the pH regulator agent is acids (example hydrochloric acid, sulfuric acid, acetic acid, a phosphoric acid etc.); When being lower than 4 before the system pH regulator, the pH regulator agent is a bases, is ammoniacal liquor of 10~15% etc. like NaOH or weight concentration;
Said ultraviolet source is a 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: with acrylic amide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent and other functional monomers is raw material; In the presence of photoinitiator; In nitrogen atmosphere with the UV-irradiation initiated polymerization; Viscosity stops irradiating ultraviolet light after reaching target zone, finishes polyreaction.Because light-initiated characteristics; Radical can produce in a short period of time; Also can disappear in a short period of time, so this method compares conventional compound method and have simple to operately, viscosity is easy to control; Advantages such as gelation can be effectively prevented, all moderate Dry Strength Resin of molecular weight, the degree of branching and viscosity can be obtained.
Through regulating the ratio of the monomeric ratio of soft or hard, zwitterion; And through adding cross-linkable monomer introducing branched structure; Make Dry Strength Resin have good performance, add the ring pressure that can improve into paper behind the paper pulp well, folding, anti-ly brokenly, anti-open, performance such as paper internal bond strength.In addition, branched structure that this Dry Strength Resin had and suitable hydrophilic and hydrophobic matter make it have less viscosity, in water, have good dispersiveness, can dilute at an easy rate, the convenient use.
Has few, the good effectiveness of consumption with present method synthetic Dry Strength Resin.Can in the production of multiple paper kinds such as boxboard, Corrugating Base Paper, enamelled paper, cop tube paper, speciality paper, use, play the effect that increases the paper dry strength, especially when starching as paper making raw material with reclaimed waste paper, effect is more remarkable.Such Dry Strength Resin can have outstanding paper and do reinforced effects under the situation of not adding Tai-Ace S 150.
Embodiment
Among the embodiment, viscosity all adopts Brookfield DV-II type viscometer determining down at 25 ℃.
Embodiment 1
. in reaction kettle, add entry 405g, acrylic amide 118g, methylene-succinic acid 2g, methylacryoyloxyethyl trimethyl ammonium chloride 16g, methylene-bisacrylamide 0.08g, sodium allyl sulfonate 1g, Propylene glycol monoacrylate 4g, ethyl propenoate 2g and UVNUL MS-40 1g and stir, reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly; Keep logical nitrogen then, temperature of reaction kettle is risen to 85 ℃, the reaction system irradiating ultraviolet light; The basic maintenance, reacted 1.5 hours under the homothermic situation; Begin afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes, viscosity stops irradiating ultraviolet light after reaching 4500mPa*s, adds liquid caustic soda (32%; Weight) 1.5g regulates pH to 4; Add Resorcinol 0.02g at last, add water and regulate weight solid content to 20%, be the finished product.
Embodiment 2.
In reaction kettle, adding entry 400g, acrylic amide 100g, methylene-succinic acid 2g, methylacryoyloxyethyl trimethyl ammonium chloride 15g, methylene-bisacrylamide 0.08g, sodium allyl sulfonate 0.8g, Propylene glycol monoacrylate 15g, vinylbenzene 5g and UVNUL MS-40 0.5g stirs; Reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly, keep logical nitrogen then, temperature of reaction kettle is risen to 75 ℃; To the reaction system irradiating ultraviolet light; The basic maintenance, reacted 2 hours under the homothermic situation, beginning afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes, and viscosity stops irradiating ultraviolet light after reaching 5000mPa*s; Add liquid caustic soda (32% weight) 1.5g and regulate pH to 6; Add sodium sulfite anhy 96 2g at last, add water and regulate solid content to 20%, be the finished product.
Embodiment 3
. in reaction kettle, add entry 410g, acrylic amide 110g, maleic anhydride 2g, (methyl) dimethylaminoethyl acrylate 10g, DMAA 0.9g, sodium allyl sulfonate 0.6g, Rocryl 410 15g, vinylbenzene 5g and UVNUL MS-40 0.7g and stir, reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly, keep logical nitrogen then; Temperature of reaction kettle is risen to 75 ℃; To the reaction system irradiating ultraviolet light, keep basically reacting 2 hours under the homothermic situation, beginning afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes; Viscosity stops irradiating ultraviolet light after reaching 5000mPa*s; Add sulfuric acid (15%, weight) and regulate pH to 5, add at last copper sulfate 0.01g; Regulate weight solid content to 20%, be the finished product.
Embodiment 4
. in reaction kettle, add entry 520g, acrylic amide 82g, methylene-succinic acid 1g, methylacryoyloxyethyl trimethyl ammonium chloride 9g, methylene-bisacrylamide 0.03g, sodium allyl sulfonate 0.2g, TEB 3K 4g, Propylene glycol monoacrylate 1g, ethyl propenoate 1g and UVNUL MS-40 0.5g successively and stir, reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly, keep logical nitrogen then; Temperature of reaction kettle is risen to 85 ℃; To the reaction system irradiating ultraviolet light, keep basically reacting 1.5 hours under the homothermic situation, beginning afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes; Viscosity stops irradiating ultraviolet light after reaching 3500mPa*s; Add liquid caustic soda (32%, weight) and regulate pH to 6, add para benzoquinone 0.01g at last; Add water and regulate weight solid content to 15%, be the finished product.
Embodiment 5
. in reaction kettle, add entry 570g, acrylic amide 82g, toxilic acid 1g, methylacryoyloxyethyl trimethyl ammonium chloride 10g, DMAA 0.5g, Thiovanic acid 0.005g, vinylbenzene 2g, Propylene glycol monoacrylate 1g, ethyl propenoate 5g and eosin 0.7g successively and stir, reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly, keep logical nitrogen then; Temperature of reaction kettle is risen to 80 ℃; To the reaction system irradiating ultraviolet light, keep basically reacting 1.5 hours under the homothermic situation, beginning afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes; Viscosity stops irradiating ultraviolet light after reaching 3500mPa*s; Add liquid caustic soda (32%, weight) and regulate pH to 5, add Resorcinol 0.01g at last; Add water and regulate weight solid content to 15%, be the finished product.
Embodiment 6.
In reaction kettle, add entry 500g, acrylic amide 80g, vinylformic acid 2g, dimethyl diallyl ammonium chloride 10g, Vinyl toluene 0.5g, sodium sulfite anhy 96 0.8g, Propylene glycol monoacrylate 1g, TEB 3K ester 5g and benzoin methyl ether 0.7g successively and stir, reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly, keep logical nitrogen then; Temperature of reaction kettle is risen to 80 ℃; To the reaction system irradiating ultraviolet light, keep basically reacting 1.5 hours under the homothermic situation, beginning afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes; Viscosity stops irradiating ultraviolet light after reaching 4500mPa*s; Add liquid caustic soda (32%, weight) and regulate pH to 4, add Resorcinol 0.01g at last; Add water and regulate weight solid content to 15%, be the finished product.
Embodiment 7.
In reaction kettle, add entry 420g, acrylic amide 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 and stir, reaction kettle is vacuumized logical nitrogen 2~3 times repeatedly, keep logical nitrogen then; Temperature of reaction kettle is risen to 82 ℃; To the reaction system irradiating ultraviolet light, keep basically reacting 2 hours under the homothermic situation, beginning afterwards whenever to carry out viscosity test at a distance from sampling in 20 minutes; Viscosity stops irradiating ultraviolet light after reaching 4500mPa*s; Add liquid caustic soda (32%, weight) and regulate pH to 6, add Dichlorodiphenyl Acetate copper 0.01g at last; Add water and regulate weight solid content to 30%, be the finished product.
Comparative example 1.
In reaction kettle, adding entry 550g, acrylic amide 81g, vinylformic acid 2g, methylacryoyloxyethyl trimethyl ammonium chloride 9g, methylene-bisacrylamide 0.1g, sodium allyl sulfonate 0.1g successively stirs; Logical nitrogen drove oxygen 60 minutes, was warmed up to 60 ℃, added ammonium persulphate 0.5g (being dissolved in the 20g water); Temperature of reaction kettle is risen to 82 ℃; React that viscosity increases sharply after 30 minutes, temperature rises rapidly, gelation behind the several minutes.
Comparative example 2.
In reaction kettle, adding entry 550g, acrylic amide 81g, vinylformic acid 2g, methylacryoyloxyethyl trimethyl ammonium chloride 9g, sodium allyl sulfonate 0.2g successively stirs; Logical nitrogen drove oxygen 60 minutes; Be warmed up to 60 ℃; Add ammonium persulphate 0.5g (being dissolved in the 20g water), temperature of reaction kettle is risen to 82 ℃, reacting begins after 1 hour to take a sample detects viscosity.Viscosity adds the stopper stopped reaction after reaching 5000mPa*s.Regulate pH to 4, adding water move to the weight solid content is 15%.
Comparative example 3.
In reaction kettle, add entry 550g, acrylic amide 81g, vinylformic acid 2g, methylacryoyloxyethyl trimethyl ammonium chloride 9g, DMAA 0.8g successively; Sodium allyl sulfonate 0.2g stirs; Logical nitrogen drove oxygen 60 minutes, was warmed up to 60 ℃, added ammonium persulphate 0.5g (being dissolved in the 20g water); Temperature of reaction kettle is risen to 82 ℃, and reacting begins after 1 hour to take a sample detects viscosity.Viscosity adds the stopper stopped reaction after reaching 3500mPa*s.Regulate pH to 6, adding water move to the weight solid content is 15%.The timed interval of viscosity between 3000mPa*s and 10000mPa*s has only 10 minutes, and be difficult with control.
Embodiment 8, application example
. adopt the reclaimed waste paper case to pull an oar as raw material; Beating degree adds Dry Strength Resin stirring 5 minutes after reaching 35 ° of SR; Employing standard page squeezing machine squeezing after semi-automatic sheet-former is shaped; Natural air drying detects the index such as tensile strength, ring crush intensity, bursting strength, folding endurance, internal bond strength of paper then.The Dry Strength Resin add-on is 6 ‰ (doing/oven dry stock).Table 2 has provided the application data of the prepared Dry Strength Resin of aforesaid method.
Table 2. adds the handsheet intensity index (doing/oven dry stock) of Dry Strength Resin
Can be known that by the foregoing description, Comparative Examples and application examples method therefor of the present invention has simple to operate, viscosity is easy to control, can effectively prevent advantages such as gelation.Have good application performance with this method institute synthetic Dry Strength Resin, compare straight chain type Dry Strength Resin (comparative example 2) and have significant advantage, comparing with general method institute synthetic branched chain type Dry Strength Resin (comparative example 3) effect has certain advantage.
The above is not that technical scheme of the present invention is done any pro forma restriction only as part embodiment of the present invention.Every technical spirit according to the present invention all still belongs to technical scheme scope of the present invention to any simple modification, equivalent variations and modification that above embodiment did.
Claims (7)
1. the preparation method of papermaking Dry Strength Resin is characterized in that, comprises the steps: in nitrogen atmosphere; With water, acrylic amide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent, other functional monomers and photoinitiator; Reaction under UV-irradiation adds the pH regulator agent and regulates pH to 4~6, adds free radical scavenger at last; Mix, obtain described papermaking Dry Strength Resin.
2. method according to claim 1 is characterized in that, 70~95 ℃ were reacted 1.5~2 hours.
3. method according to claim 1 and 2 is characterized in that, raw materials in part by weight is:
4. method according to claim 3; It is characterized in that said cationic monomer is that (methyl) acrylyl oxy-ethyl-trimethyl salmiac, (methyl) dimethylaminoethyl acrylate, (methyl) vinylformic acid lignocaine ethyl ester, diallyldimethylammonium chloride, dimethylamino propyl acrylamide etc. are with one or more in uncle's amino monomers or the quaternary ammonium salt monomer;
Said anionic monomer is one or more in monomers such as vinylformic acid, methylacrylic 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;
Said cross-linkable monomer is that di-vinyl monomers, trivinyl monomer or other have active monomer;
Said other functional monomers are Hydroxyethyl acrylate, Propylene glycol monoacrylate, vinylbenzene, TEB 3K, alkyl acrylate or alkyl methacrylate;
Said free radical scavenger is various water-soluble stoppers, and preferably Resorcinol, benzoquinones, iron(ic)chloride, neutralized verdigris etc. maybe can consume the material of radical, like sodium sulfite anhy 96 or xitix etc.;
Said ultraviolet source is a high voltage mercury lamp, and its wavelength is 100~1000nm, and its power is according to the size adjustment of reaction vessel.
5. method according to claim 4 is characterized in that, other have active monomer is N, the N-DMAA.
6. method according to claim 3 is characterized in that, said photoinitiator is UVNUL MS-40, UVNUL MS-40 soluble derivative, st-yrax analog derivative, resorcinolphthalein or eosin;
Said chain-transfer agent is other materials, the Virahol of sodium sulfite anhy 96, Sodium Pyrosulfite, Sulfothiorine, positive Dodecyl Mercaptan, tert-dodecyl mercaptan, Thiovanic acid, mercaptoethanol, band sulfydryl or has in the allylic monomer one or more;
Said pH regulator agent confirms that as the case may be when being higher than 6 before the system pH regulator, the pH regulator agent is hydrochloric acid, sulfuric acid, acetic acid, phosphoric acid; When being lower than 4 before the system pH regulator, the pH regulator agent is that NaOH or weight concentration are 10~15% ammoniacal liquor.
7. the papermaking Dry Strength Resin for preparing according to each said method of claim 1~6.
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CN109180861A (en) * | 2018-08-21 | 2019-01-11 | 上海昶法新材料有限公司 | A kind of novel drying strengthening agent 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 |
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