CN102617791A - Amphoteric dry strength agent and preparation method thereof - Google Patents
Amphoteric dry strength agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an amphoteric dry strength agent and a preparation method thereof. The preparation method comprises the following steps: in a nitrogen atmosphere, the mixture of water, acrylamide, anionic monomer, cationic monomer, cross-link monomer, a chain transfer agent and other functional monomer and photoinitiator is subjected to ultraviolet irradiation reaction; pH regulator is added to adjust a pH value after the reaction is finished; and free radical catcher is added to obtain the product. The anionic monomer is the mixture of itaconate and sodium vinylsulfonate with the mass ratio of 1 to (3 to 5); the cationic monomer is the mixture of acrylic acid lignocaine ethyl ester and diallyl dimethyl ammonium chloride with the mass ratio of 1 to (2 to 3); and the functional monomer is the mixture of styrene and hydroxyethyl acrylate with the mass ratio of 1 to (1.5 to 3.5). The amphoteric dry strength agent has the characteristics of small dosage and good effect; particularly, when reclaimed waste paper pulp is adopted as papermaking raw material, the effect is more remarkable; and an excellent paper dry-strengthening effect is achieved under the condition that no aluminium sulphate is added.
Description
Technical field
The present invention relates to increase in a kind of paper industry the preparation method of paper strength both sexes Dry Strength Resin.
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 both sexes 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; Mixture with water, acrylic amide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent, other functional monomers and photoinitiator; Under UV-irradiation, 70～95 ℃ were reacted 1.5～2 hours, and reaction finishes the back and adds pH regulator agent adjusting pH to 4～6; Add free radical scavenger at last, obtain product;
Proportioning raw materials in the above process step (is all calculated with effective content 100% by weight, raw material) as follows:
Said cationic monomer is selected from one or more in band such as (methyl) acrylyl oxy-ethyl-trimethyl salmiac, (methyl) dimethylaminoethyl acrylate, (methyl) vinylformic acid lignocaine ethyl ester, diallyldimethylammonium chloride, dimethylamino propyl acrylamide uncle amino monomers, the quaternary ammonium salt monomers, and the preferred cation monomer is vinylformic acid lignocaine ethyl ester and the diallyldimethylammonium chloride mixture by mass ratio 1: 2～3.Adding cationic monomer unit can make Dry Strength Resin and paper-making fibre have better bonding force.
Said anionic monomer can be selected from monomer or its salt such as vinylformic acid, methylacrylic acid, methylene-succinic acid, toxilic acid, fumaric acid, maleic anhydride, sodium vinyl sulfonate, vinylbenzenesulfonic acid sodium, sodium allyl sulfonate and methallylsulfonic acid sodium, preferred methylene-succinic acid and sodium vinyl sulfonate are pressed mass ratio 1: 3～5 mixture; 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 (like N, N-diallyl acrylic amide etc.) or other have one or more in the active monomer (like N, N-DMAA etc.).The participation of cross-linkable monomer can make polymkeric substance produce side chain at an easy rate.
Said functional monomer can be in some soft monomers (like Hydroxyethyl acrylate, Propylene glycol monoacrylate), hard monomer (like vinylbenzene, TEB 3K), the hydrophobic monomer (like alkyl acrylate, alkyl methacrylate etc.) one or more, optimization styrene and Hydroxyethyl acrylate are pressed mass ratio 1: 1.5～3.5 mixture.Various 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 and eosin etc.
Said chain-transfer agent can and have in the allylic monomer one or more for 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.).
Said free radical scavenger is the material (like sodium sulfite anhy 96, xitix etc.) that various water-soluble stoppers (like Resorcinol, benzoquinones, iron(ic)chloride, neutralized verdigris etc.) maybe can consume radical.
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 bases (like NaOH, an ammoniacal liquor 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.
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
Embodiment 1
In reaction kettle, add entry 405g, acrylic amide 118g, methylene-succinic acid 3g, sodium vinyl sulfonate 15g, methylene-bisacrylamide 0.08g, vinylformic acid lignocaine ethyl ester 0.3g, diallyldimethylammonium chloride 0.7g, Hydroxyethyl acrylate 4g, vinylbenzene 2g and UVNUL MS-40 1g 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, add liquid caustic soda (32%; Weight) 1.5g regulates pH to 6; 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 successively 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, adds liquid caustic soda (32% weight) 1.5g and regulate pH to 4, adds sodium sulfite anhy 96 2g at last; Add water and regulate weight solid content to 20%, be the finished product.
Embodiment 3
In reaction kettle, adding 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 successively 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, adds sulfuric acid (15% weight) and regulate pH to 5, adds at last copper sulfate 0.01g; Regulate weight solid content to 20%, be the finished product.
Embodiment 4
In reaction kettle, adding 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 stirs; 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; The basic maintenance, reacted 1.5 hours under the homothermic situation, adds liquid caustic soda (32% weight) and regulate pH to 6, adds para benzoquinone 0.01g at last; Add water and regulate weight solid content to 15%, be the finished product.
Embodiment 5
In reaction kettle, adding 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 stirs; 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; The basic maintenance, reacted 1.5 hours under the homothermic situation, adds liquid caustic soda (32% weight) and regulate pH to 4, adds Resorcinol 0.01g at last; Add water and regulate weight solid content to 15%, be the finished product.
Embodiment 6
In reaction kettle, adding 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 stirs; 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; The basic maintenance, reacted 1.5 hours under the homothermic situation, adds liquid caustic soda (32% weight) and regulate pH to 6, adds Resorcinol 0.01g at last; Add water and regulate weight solid content to 15%, be the finished product.
Embodiment 7
In reaction kettle, adding 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 successively stirs; 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; The basic maintenance, reacted 2 hours under the homothermic situation, adds liquid caustic soda (32% weight) and regulate pH to 5, adds 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, 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 ℃, react adding stopper stopped reaction after 1 hour.Regulate pH to 6, adding water move to the weight solid content is 15%.
Embodiment 8
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 4.5～7.5 ‰ (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.
Claims (7)
1. the preparation method of a both sexes Dry Strength Resin is characterized in that, comprises the steps: in nitrogen atmosphere; Mixture with water, acrylic amide, anionic monomer, cationic monomer, cross-linkable monomer, chain-transfer agent, other functional monomers and photoinitiator; Under UV-irradiation, 70～95 ℃ were reacted 1.5～2 hours, and reaction finishes the back and adds pH regulator agent adjusting pH to 4～6; Add free radical scavenger at last, obtain product;
Said anionic monomer is methylene-succinic acid and the sodium vinyl sulfonate mixture by mass ratio 1: 3～5; Said cationic monomer is vinylformic acid lignocaine ethyl ester and the diallyldimethylammonium chloride mixture by mass ratio 1: 2～3; Said functional monomer is vinylbenzene and the Hydroxyethyl acrylate mixture by mass ratio 1: 1.5～3.5.
2. method according to claim 1 is characterized in that, raw material weight umber proportioning is following:
3. method according to claim 2 is characterized in that, said cross-linkable monomer is methylene-bisacrylamide, N, N-diallyl acrylic amide or N, one or more in the N-DMAA;
Said functional monomer is one or more in Hydroxyethyl acrylate, Propylene glycol monoacrylate, vinylbenzene, TEB 3K, alkyl acrylate or the alkyl methacrylate.
4. method according to claim 3 is characterized in that, said functional monomer is vinylbenzene and the Hydroxyethyl acrylate mixture by mass ratio 1: 1.5～3.5.
5. method according to claim 2 is characterized in that, said photoinitiator is UVNUL MS-40, UVNUL MS-40 soluble derivative, st-yrax analog derivative, resorcinolphthalein or eosin etc.;
Said chain-transfer agent is other materials, the Virahol of sodium sulfite anhy 96, Sodium Pyrosulfite, sodium thiosulfate, positive Dodecyl Mercaptan, tert-dodecyl mercaptan, Thiovanic acid, mercaptoethanol, band sulfydryl or in the allylic monomer one or more is arranged;
Said free radical scavenger is Resorcinol, benzoquinones, iron(ic)chloride, neutralized verdigris, sodium pyrosulfate or xitix.
6. method according to claim 2 is characterized in that, said pH regulator agent is acid, sulfuric acid, acetic acid, phosphoric acid, NaOH or ammoniacal liquor.
7. the both sexes Dry Strength Resin for preparing according to each said method of claim 1～6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408701A (en) * | 2013-07-09 | 2013-11-27 | 上海东升新材料有限公司 | Method for preparing dry strength agent by ultraviolet-initiated polymerization |
| 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 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20090030542A (en) * | 2007-09-20 | 2009-03-25 | 주식회사 화성산업 | Dry strength agent of cation block type and producing method thereof |
| CN102115998A (en) * | 2010-12-31 | 2011-07-06 | 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 |
| CN102121207A (en) * | 2010-12-03 | 2011-07-13 | 江门市高力依科技实业有限公司 | Papermaking dry-strengthening agent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20090030542A (en) * | 2007-09-20 | 2009-03-25 | 주식회사 화성산업 | Dry strength agent of cation block type and producing method thereof |
| CN102121207A (en) * | 2010-12-03 | 2011-07-13 | 江门市高力依科技实业有限公司 | Papermaking dry-strengthening agent |
| CN102115998A (en) * | 2010-12-31 | 2011-07-06 | 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103408701A (en) * | 2013-07-09 | 2013-11-27 | 上海东升新材料有限公司 | Method for preparing dry strength agent by ultraviolet-initiated polymerization |
| 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 |
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