CN102660903B - Preparation method for soap-free polymer anionic alkyl ketene dimer (AKD) neutral/alkaline sizing agent - Google Patents
Preparation method for soap-free polymer anionic alkyl ketene dimer (AKD) neutral/alkaline sizing agent Download PDFInfo
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229920000642 polymer Polymers 0.000 title abstract description 8
- 125000000217 alkyl group Chemical group 0.000 title abstract description 3
- 230000007935 neutral effect Effects 0.000 title abstract 3
- 125000000129 anionic group Chemical group 0.000 title abstract 2
- WASQWSOJHCZDFK-UHFFFAOYSA-N diketene Chemical compound C=C1CC(=O)O1 WASQWSOJHCZDFK-UHFFFAOYSA-N 0.000 title abstract 2
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 80
- 239000000839 emulsion Substances 0.000 claims abstract description 51
- 239000003999 initiator Substances 0.000 claims abstract description 43
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 31
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 30
- IVKNZCBNXPYYKL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[4-(2,4,4-trimethylpentan-2-yl)phenoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CC(C)(C)CC(C)(C)C1=CC=C(OCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO)C=C1 IVKNZCBNXPYYKL-UHFFFAOYSA-N 0.000 claims abstract description 29
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 29
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims abstract description 18
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 15
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 15
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 3
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 46
- 150000001768 cations Chemical class 0.000 claims description 45
- 239000000243 solution Substances 0.000 claims description 43
- 239000011259 mixed solution Substances 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- 238000006243 chemical reaction Methods 0.000 claims description 31
- 229960000583 acetic acid Drugs 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 28
- 238000010792 warming Methods 0.000 claims description 28
- 239000003643 water by type Substances 0.000 claims description 24
- 238000013019 agitation Methods 0.000 claims description 14
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- 238000002844 melting Methods 0.000 claims description 14
- 230000008018 melting Effects 0.000 claims description 14
- DYUWTXWIYMHBQS-UHFFFAOYSA-N n-prop-2-enylprop-2-en-1-amine Chemical compound C=CCNCC=C DYUWTXWIYMHBQS-UHFFFAOYSA-N 0.000 claims description 14
- 229940079827 sodium hydrogen sulfite Drugs 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 150000000211 1-dodecanols Chemical class 0.000 claims description 12
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 230000014759 maintenance of location Effects 0.000 abstract description 3
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- -1 polyethylene Polymers 0.000 abstract description 3
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- YRMLFORXOOIJDR-UHFFFAOYSA-N Dichlormid Chemical compound ClC(Cl)C(=O)N(CC=C)CC=C YRMLFORXOOIJDR-UHFFFAOYSA-N 0.000 abstract 1
- 239000004698 Polyethylene Substances 0.000 abstract 1
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000007334 copolymerization reaction Methods 0.000 abstract 1
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- 230000020477 pH reduction Effects 0.000 abstract 1
- 229920000573 polyethylene Polymers 0.000 abstract 1
- 150000003254 radicals Chemical class 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 239000007844 bleaching agent Substances 0.000 description 7
- 239000011436 cob Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000000835 fiber Substances 0.000 description 6
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- 238000004945 emulsification Methods 0.000 description 3
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- NJVOHKFLBKQLIZ-UHFFFAOYSA-N (2-ethenylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C=C NJVOHKFLBKQLIZ-UHFFFAOYSA-N 0.000 description 1
- 235000004258 Cordia alliodora Nutrition 0.000 description 1
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- 241000276489 Merlangius merlangus Species 0.000 description 1
- 241000533901 Narcissus papyraceus Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
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Abstract
The invention discloses a preparation method for a soap-free polymer anionic alkyl ketene dimer (AKD) neutral/alkaline sizing agent. The preparation method comprises the following steps of: preparing a reactive emulsifier from raw materials OP-10, maleic anhydride and dodecanol, performing free radical copolymerization reaction on the reactive emulsifier, styrene, ethyl acrylate and dichlormid by taking ammonium persulfate and sodium bisulfite as initiators and taking dodecanethiol as a molecular weight regulator, and performing acidification by using acetic acid to obtain a polymer, wherein the polymer can be used as an AKD emulsifier, an AKD emulsion stabilizer and a sizing synergist, and is applied to the emulsion of polyethylene wax and AKD as an emulsifier. Prepared neutral/alkaline sizing emulsion particles are positively charged under an acidic condition, and have high emulsion and dispersion capabilities, high retention and good sizing effects, and the sizing degree is remarkably improved.
Description
Technical field
The invention belongs to polymer chemistry sizing agent field, the preparation method of particularly in a kind of soap-free polymerization thing cation AKD/alkaline sizing agent.
Background technology
The major progress of modern applying glue technology be in/popularization of alkaline bleach liquor sizing technology, during acid papermaking is converted into/alkaline paper-making is the great change in world's papermaking history.In/alkaline bleach liquor sizing is in papermaking process, pH value is adjusted to more than 7, in principle without a kind of glue applying method of aluminum sulfate.In conventional/alkaline sizing agent alkyl ketene dimer (being called for short AKD) is the product of phase late 1940s research and development, AKD be a kind of can with the response type of fibrin reaction in/alkaline sizing agent, it can serve as internal sizing agent, can serve as again Cypres.Its design feature is to be made up of active group and hydrophobic grouping, the fusing point of AKD is lower, hydroxyl reaction on active group quaternary lactonic ring energy and cellulose under the hot conditions of Dryer Section of Paper Machine in molecule forms beta-keto ester bond and is positioned on fiber, and hydrophobic group chain alkyl produces water resistant effect at fiber surface.By in AKD/alkaline bleach liquor sizing, the one way retention of Paper White Degree, feel, WATER RESISTANCE, physical strength, printability, resistance to ag(e)ing and filler etc. is all significantly improved.And can to adopt cheap powdered whiting be filler, reduce the content of harmful substance in plain boiled water, improve the cyclic utilization rate of plain boiled water, AKD is lower than the cost of acid accumulator size simultaneously.Adopt AKD carry out in/alkaline bleach liquor sizing can improve paper product quality and price, reduction energy consumption, improve environmental pollution and paper machine operation performance etc., can obtain obvious economic benefit and social benefit, therefore increasing papermaking enterprise is recognized superiority and the necessity of use in AKD/alkaline sizing agent.China's paper making raw material is taking straw pulp as main, timber resource shortage, and secondary stock consumption increases, in utilization/alkaline bleach liquor sizing technology has realistic meaning.Follow in AKD/alkaline bleach liquor sizing technology progressively expands in China's Application Areas, technology is increasingly mature, in/benefit of alkaline paper-making progressively embodied, accelerated paper industry by acid papermaking in/trend that alkaline paper-making changes, in recent years AKD become domestic paper plant use at most, the most ripe, the most effectively in/alkaline sizing agent.
In AKD/alkaline bleach liquor sizing gives paper some excellent properties, also has its weak point simultaneously.AKD is unstable in water, AKD emulsion preparation and deposit in process easily hydrolysis and lost efficacy.When wet paper page drying position, the time that AKD at high temperature contact with water is longer, and AKD reacts with fiber and AKD vies each other with the hydrolysis that water carries out, and part AKD, because of hydrolysis inefficacy, causes degree of sizing decline or hysteresis.Improve in recent years and to improve the research of AKD emulsion property increasingly active, reduce the hydrolysis of AKD, improve the extent of reaction of AKD and fiber, development and production good emulsion stability and with the active high AKD emulsion of fiber-reactive be that China's papermaking researcher is made great efforts the problem of studying always.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the preparation method of the object of the present invention is to provide in a kind of soap-free polymerization thing cation AKD/alkaline sizing agent, in gained/alkaline sizing agent hydrolysis, there is good storage stability, also there is high reactivity even if there is water to exist under hot environment, thereby greatly improved reaction efficiency and the sizing efficiency of sizing material.
For achieving the above object, the technical solution used in the present invention is:
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, comprise following concrete steps:
The first step, OP-10 and maleic anhydride are added in the first reactor and to react 1.0-1.5 hour 75-80 DEG C time, then add lauryl alcohol in 90-95 DEG C of reaction 2.0-2.5 hour, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by reactive emulsifier, styrene, ethyl acrylate, diallylamine and lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by ammonium persulfate, sodium hydrogensulfite and deionized water with mass ratio at 2: 1: 30,
The 4th step adds deionized water in the second reactor, is warming up to 55-65 DEG C, adds respectively initiator solution and mixed solution, and the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.0-1.5 hour,
The 5th step, reinforced after in 80-90 DEG C of insulation reaction 2.0-3.0 hour,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value, to 4-5, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add AKD emulsifying agent, Tissuemat E and AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 120-130 DEG C, after AKD melting, stir 40-50 minute, then under agitation add the deionized water of 70-80 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 20-30MPa homogeneous, be cooled to room temperature,, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent to 4-5 with vinegar acid for adjusting pH value.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 65-75 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 7.5-8.5, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 4.0-6.5Kg/t paper, after lower machine, the Cobb value of wood-free paper is 27-32g/m
2, and save sizing material 22-27%.
The present invention does not adopt low molecule emulsifying agent in preparation process, and reactive emulsifier becomes a part for strand in polymerization process with covalent bonds, thereby has eliminated the weak point that low molecule emulsifying agent brings.The polymer obtaining is the emulsifying agent of AKD, again stabilizing agent and the sizing synergist of AKD emulsion, set it as the emulsification that emulsifying agent is applied to Tissuemat E and AKD, in preparation/alkaline sizing agent emulsion particle is positively charged under acid condition, there is stronger emulsification and dispersibility, can AKD be carried out effective emulsification and fully be disperseed, obtain having the sizing agent emulsion of good stability.In paper-making process, (in/alkali condition) stabilizing agent lost efficacy, and was conducive to AKD and the cellulose generation degree of sizing that reacts, and this is the improvement greatly to starch series AKD emulsion emulsifying technology.
Detailed description of the invention
Below will with specific embodiment, the present invention is described in further detail.
Embodiment mono-
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, specifically comprise the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.5 hours 75 DEG C time, then add 10 grams of lauryl alcohols in 90 DEG C of reactions 2.5 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 55 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.5 hours
The 5th step, reinforced after in 80 DEG C of insulation reaction 3.0 hours,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value to 4, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 120 DEG C, after AKD melting, stir 50 minutes, then under agitation add the deionized water of 70 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 20MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 65 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 7.5, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 4.0Kg/t paper, after lower machine, the Cobb value of wood-free paper is 32g/m
2, and save sizing material 27%.
Embodiment bis-
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, specifically comprise the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.4 hours 76 DEG C time, then add 10 grams of lauryl alcohols in 91 DEG C of reactions 2.4 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 57 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.4 hours
The 5th step, reinforced after in 82 DEG C of insulation reaction 2.8 hours,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value to 4.2, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 122 DEG C, after AKD melting, stir 48 minutes, then under agitation add the deionized water of 72 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 22MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.2, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 67 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 7.7, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 4.5Kg/t paper, after lower machine, the Cobb value of wood-free paper is 31g/m
2, and save sizing material 26%.
Embodiment tri-
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, specifically comprise the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.3 hours 77 DEG C time, then add 10 grams of lauryl alcohols in 92 DEG C of reactions 2.3 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 59 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.3 hours
The 5th step, reinforced after in 84 DEG C of insulation reaction 2.6 hours,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value to 4.4, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 124 DEG C, after AKD melting, stir 46 minutes, then under agitation add the deionized water of 74 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 24MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.4, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 69 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 7.9, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 5.0Kg/t paper, after lower machine, the Cobb value of wood-free paper is 30g/m
2, and save sizing material 25%.
Embodiment tetra-
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, specifically comprise the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.2 hours 78 DEG C time, then add 10 grams of lauryl alcohols in 93 DEG C of reactions 2.2 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 61 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.2 hours
The 5th step, reinforced after in 86 DEG C of insulation reaction 2.4 hours,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value to 4.6, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 126 DEG C, after AKD melting, stir 44 minutes, then under agitation add the deionized water of 76 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 26MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.6, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 71 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 8.1, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 5.5Kg/t paper, after lower machine, the Cobb value of wood-free paper is 29g/m
2, and save sizing material 24%.
Embodiment five
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, specifically comprise the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.1 hours 79 DEG C time, then add 10 grams of lauryl alcohols in 94 DEG C of reactions 2.1 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 63 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.1 hours
The 5th step, reinforced after in 88 DEG C of insulation reaction 2.2 hours,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value to 4.8, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 128 DEG C, after AKD melting, stir 42 minutes, then under agitation add the deionized water of 78 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 28MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.8, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 73 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 8.3, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 6.0Kg/t paper, after lower machine, the Cobb value of wood-free paper is 28g/m
2, and save sizing material 23%.
Embodiment six
In soap-free polymerization thing cation AKD/and the preparation method of alkaline sizing agent, specifically comprise the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.0 hours 80 DEG C time, then add 10 grams of lauryl alcohols in 95 DEG C of reactions 2.0 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 65 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.0 hours
The 5th step, reinforced after in 90 DEG C of insulation reaction 2.0 hours,
The 6th step, is down to greenhouse, and with vinegar acid for adjusting pH value to 5, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 130 DEG C, after AKD melting, stir 40 minutes, then under agitation add the deionized water of 80 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 30MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 5, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
In the soap-free polymerization thing cation AKD obtaining with the present invention/the emulsion extension of validity of alkaline sizing agent 75 days, use it for 70g/m
2in the plasm-glue-blending of wood-free paper, pH value is 8.5, in soap-free polymerization thing cation AKD/alkaline sizing agent consumption 6.5Kg/t paper, after lower machine, the Cobb value of wood-free paper is 27g/m
2, and save sizing material 22%.
In sum, the present invention adopts reactive emulsifier and styrene-acrylate to carry out copolyreaction, obtain cationic amine based polymer and replace the emulsion stabilizer of cationic starch as AKD, its positive electricity density is easy to adjust, the positive electricity adaptability of AKD micelle cohesion is strengthened, form the AKD sizing agent that is applicable to special wet end environment.Amine polymer has reduced hydrolysis tendency effectively to the adjustment of AKD emulsion particle electric charge, and makes the extension of validity of AKD emulsion.This emulsion has increased the affinity of AKD molecule and cellulose hydroxyl, improve keeping on fiber, AKD particulate even also can be combined with fibre compact in the situation that paper moisture content increases, and therefore degree of sizing obviously improves, and has good retention and sizing efficiency.
Claims (7)
1. the preparation method of in 1 one kinds of soap-free polymerization thing cation AKDs of claim/alkaline sizing agent, is characterized in that, comprises following concrete steps:
The first step, OP-10 and maleic anhydride are added in the first reactor and to react 1.0-1.5 hour 75-80 DEG C time, then add lauryl alcohol in 90-95 DEG C of reaction 2.0-2.5 hour, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by reactive emulsifier, styrene, ethyl acrylate, diallylamine and lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by ammonium persulfate, sodium hydrogensulfite and deionized water with mass ratio at 2: 1: 30,
The 4th step adds deionized water in the second reactor, is warming up to 55-65 DEG C, adds respectively initiator solution and mixed solution, and the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.0-1.5 hour,
The 5th step, reinforced after in 80-90 DEG C of insulation reaction 2.0-3.0 hour,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value, to 4-5, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add AKD emulsifying agent, Tissuemat E and AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 120-130 DEG C, after AKD melting, stir 40-50 minute, then under agitation add the deionized water of 70-80 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 20-30MPa homogeneous, be cooled to room temperature,, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent to 4-5 with vinegar acid for adjusting pH value.
2. the preparation method of in a kind of soap-free polymerization thing cation AKD according to claim 1/alkaline sizing agent, is characterized in that, specifically comprises the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.5 hours 75 DEG C time, then add 10 grams of lauryl alcohols in 90 DEG C of reactions 2.5 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 55 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.5 hours
The 5th step, reinforced after in 80 DEG C of insulation reaction 3.0 hours,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value to 4, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 120 DEG C, after AKD melting, stir 50 minutes, then under agitation add the deionized water of 70 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 20MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
3. the preparation method of in a kind of soap-free polymerization thing cation AKD according to claim 1/alkaline sizing agent, is characterized in that, specifically comprises the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.4 hours 76 DEG C time, then add 10 grams of lauryl alcohols in 91 DEG C of reactions 2.4 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 57 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.4 hours
The 5th step, reinforced after in 82 DEG C of insulation reaction 2.8 hours,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value to 4.2, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 122 DEG C, after AKD melting, stir 48 minutes, then under agitation add the deionized water of 72 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 22MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.2, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
4. the preparation method of in a kind of soap-free polymerization thing cation AKD according to claim 1/alkaline sizing agent, is characterized in that, specifically comprises the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.3 hours 77 DEG C time, then add 10 grams of lauryl alcohols in 92 DEG C of reactions 2.3 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 59 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.3 hours
The 5th step, reinforced after in 84 DEG C of insulation reaction 2.6 hours,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value to 4.4, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 124 DEG C, after AKD melting, stir 46 minutes, then under agitation add the deionized water of 74 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 24MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.4, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
5. the preparation method of in a kind of soap-free polymerization thing cation AKD according to claim 1/alkaline sizing agent, is characterized in that, specifically comprises the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.2 hours 78 DEG C time, then add 10 grams of lauryl alcohols in 93 DEG C of reactions 2.2 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 61 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.2 hours
The 5th step, reinforced after in 86 DEG C of insulation reaction 2.4 hours,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value to 4.6, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 126 DEG C, after AKD melting, stir 44 minutes, then under agitation add the deionized water of 76 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 26MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.6, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
6. the preparation method of in a kind of soap-free polymerization thing cation AKD according to claim 1/alkaline sizing agent, is characterized in that, specifically comprises the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.1 hours 79 DEG C time, then add 10 grams of lauryl alcohols in 94 DEG C of reactions 2.1 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 63 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.1 hours
The 5th step, reinforced after in 88 DEG C of insulation reaction 2.2 hours,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value to 4.8, with 120 order net filtrations, discharging, obtains AKD emulsifying agent
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 128 DEG C, after AKD melting, stir 42 minutes, then under agitation add the deionized water of 78 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 28MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 4.8, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
7. the preparation method of in a kind of soap-free polymerization thing cation AKD according to claim 1/alkaline sizing agent, is characterized in that, specifically comprises the following steps:
The first step, 30 grams of OP-10 and 6 grams of maleic anhydrides are added in the first reactor and to react 1.0 hours 80 DEG C time, then add 10 grams of lauryl alcohols in 95 DEG C of reactions 2.0 hours, obtain reactive emulsifier, the mass ratio of OP-10, maleic anhydride and lauryl alcohol is 30: 6: 10
Second step, by 29 grams of reactive emulsifiers, 11 grams of styrene, 11 grams of ethyl acrylates, 8 grams of diallylamine and 1 gram of lauryl mercaptan with mass ratio 29: 11: 11: make mixed solution at 8: 1,
The 3rd step, makes initiator solution by 2 grams of ammonium persulfates, 1 gram of sodium hydrogensulfite and 30 grams of deionized waters with mass ratio at 2: 1: 30,
The 4th step adds 159 grams of deionized waters in the second reactor, is warming up to 65 DEG C, add respectively 33 grams of initiator solutions and 60 grams of mixed solutions, the mass ratio of deionized water, initiator solution and mixed solution is 159: 33: 60, and whole feed time is 1.0 hours
The 5th step, reinforced after in 90 DEG C of insulation reaction 2.0 hours,
The 6th step, is down to room temperature, and with vinegar acid for adjusting pH value to 5, with 120 order net filtrations, discharging, obtains AKD emulsifying agent,
The 7th step, in the 3rd reactor, add 145 grams of AKD emulsifying agents, 110 grams of Tissuemat Es and 145 grams of AKD, the mass ratio of AKD emulsifying agent, Tissuemat E and AKD is 145: 110: 145, be warming up to 130 DEG C, after AKD melting, stir 40 minutes, then under agitation add the deionized water of 80 DEG C to regulate solid content to 12.5%, make the sub-stable emulsion of AKD, by sub-stable emulsion after 30MPa homogeneous, be cooled to room temperature, with vinegar acid for adjusting pH value to 5, obtain solid content and be in 12.5% stable soap-free polymerization thing cation AKD/alkaline sizing agent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5438087A (en) * | 1989-12-28 | 1995-08-01 | Japan Pmc Corporation | Paper sizing composition |
| CN101649581A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Method for preparing amphoteric high molecular base AKD emulsion |
| CN101649584A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Method for preparing surface coating reinforcing agent for secondary fibre paper |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5438087A (en) * | 1989-12-28 | 1995-08-01 | Japan Pmc Corporation | Paper sizing composition |
| CN101649581A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Method for preparing amphoteric high molecular base AKD emulsion |
| CN101649584A (en) * | 2009-09-01 | 2010-02-17 | 陕西科技大学 | Method for preparing surface coating reinforcing agent for secondary fibre paper |
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Effective date of registration: 20201217 Address after: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd. Address before: 710021 Shaanxi province Xi'an Weiyang university campus of Shaanxi University of Science and Technology Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Effective date of registration: 20201217 Address after: 224000 Qingyang Road (within Qingdun Office), Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (8) Patentee after: Yancheng Qinglong Jinbang water Co.,Ltd. Address before: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd. |
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Correction item: Patentee|Address Correct: Yancheng Qingdun Jinbang Water Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8) False: Yancheng Qingyi Jinbang Water Affairs Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8) Number: 53-01 Volume: 36 |
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Granted publication date: 20140702 |