CN101324042A - Preparation of cation AKD maturing promotor - Google Patents
Preparation of cation AKD maturing promotor Download PDFInfo
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- CN101324042A CN101324042A CNA2008100231689A CN200810023168A CN101324042A CN 101324042 A CN101324042 A CN 101324042A CN A2008100231689 A CNA2008100231689 A CN A2008100231689A CN 200810023168 A CN200810023168 A CN 200810023168A CN 101324042 A CN101324042 A CN 101324042A
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Abstract
The invention discloses a preparation method for cation AKD curing accelerator which is green and protects the environment during the production process, is easy to realize the industrialization and can prompt the AKD curing, comprising the steps as follows: solvent A and monomer B are added in a polymerization device; under a condition of fast mixing and a polymerization temperature, water solution of diallyl dimethyl ammonium chloride is added; according to the gradient flux, initiator is dropped; subsequently, the polymerization temperature is kept constant for 0-120 minutes and promoter C is added and the solution is then mixed for 30 minutes; the temperature is reduced to below 10-80 DEG C and the pH value is adjusted to 1.0-7.0; the finished product is obtained by uniform mixing. The obtained product can improve the stability of AKD latex, quicken the curing speed of the AKD in the sizing process, avoid the migration of AKD, improve the antibacterial ability of the AKD latex, and can replace or partly replace the cation amylum and glitter powders.
Description
Technical field
The present invention relates to a kind of preparation method of cation AKD maturing promotor.
Background technology
Along with popularizing of neutral and alkali machine hand skill, the neutral and alkali sizing agent that matches has with it also obtained extensive use.Most important kind is exactly a reactive sizing agent in the neutral and alkali sizing agent---and alkyl ketene dimer (is called for short: AKD), about about 250,000 tons/year of present domestic consumption, there are two big defectives in AKD in the applying glue process: AKD chance water is easily degraded on the one hand, thereby lose reactivity, the AKD practical efficiency is descended, and the loss that causes because of hydrolysis is about about 30%; AKD applying glue speed is slow on the other hand, and machine slaking rate is low under the paper, has a strong impact on paper motor speed and utilization rate of equipment and installations.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method that a kind of cation AKD maturing promotor will be provided, with the product that this method makes, can improve the stability of AKD emulsion, quicken the slaking speed of AKD in the applying glue process, avoid the migration of AKD, improved AKD emulsion antibacterial ability.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of described cation AKD maturing promotor, comprise the steps: in polyplant, to add solvent orange 2 A and monomers B, stirring is warming up to 60-150 ℃ polymerization temperature, drip the aqueous solution and the initiator solution of dimethyl diallyl ammonium chloride simultaneously, dimethyl diallyl ammonium chloride is controlled at time t1 and at the uniform velocity drips off in 0-120 minute, initiator solution is controlled in 5 hours and drips off, it is constant in above-mentioned polymerization temperature 0-120 minute to drip off the back, add auxiliary agent C, stirred 10-120 minute, be cooled to below 10-80 ℃, regulating the pH value is 1.0-7.0, and stirring gets product.
Above-mentioned solvent orange 2 A is at least a in the mixture of washings, water-miscible organic solvent and water after deionized water, running water, the preceding batch of production, and the quality sum of water is no less than 50% of the total amount that feeds intake in the solvent gross mass and the dimethyl diallyl ammonium chloride aqueous solution; Above-mentioned water-miscible organic solvent is meant the water-soluble organic compounds that contains aerobic or nitrogen element, and the quality of water-miscible organic solvent is not more than 5% of the total amount that feeds intake;
Above-mentioned monomers B is selected from least a in the unsaturated fatty alcohol, and the percentage that the mole consumption of monomers B accounts for dimethyl diallyl ammonium chloride mole consumption is 0.001%-30%;
Dimethyl diallyl ammonium chloride content is at least 50% in the above-mentioned dimethyl diallyl ammonium chloride aqueous solution, is not more than 75%;
Described initiator solution is the aqueous solution of azo-compound, and the initator mass content in the initiator solution is not more than 10%; The weight ratio of initator and dimethyl diallyl ammonium chloride is between 0.0001 to 0.1; Azo-compound is selected from: azo diisopropyl imidazoline salt hydrochlorate, 2,2 '-azo (2-methyl-propyl amidine) dihydrochloride, 4, at least a in 4 '-azo (4-cyanopentanoic acid), azo diimidazole quinoline base propane dithionate, azo diisopropyl (N-3-propionyloxy) amidine hydrochloride, azo diisopropyl (N-ethoxy) imidazoline salt hydrochlorate, the azo diisopropyl imidazoline.
Described auxiliary agent C is the aqueous solution of inorganic salts, can be selected from: the aqueous solution of aluminum sulfate, aluminium chloride, aluminium polychloride, preferably sulfuric acid aluminium; The consumption of auxiliary agent C is controlled at the 0.01-10% of gained finished product total amount, preferred 1-5%.
Above-mentioned polymerization temperature is preferably 80-120 ℃.
Above-mentioned time t1 is excellent to be 0-60 minute.
For solving described technical problem better, the further technical scheme that the present invention adopts is: the rate of addition of above-mentioned initiator solution changes in gradient, that is: rate of addition increases gradually, and the initator mole flow velocity after per 20 minutes increases 1.0-2.0 doubly.
The invention has the beneficial effects as follows: the cationic polymer that a kind of production process environmental protection is provided, has been easy to realize industrialization, can promotes the AKD slaking.The products obtained therefrom effect is good, cheap, can effectively improve the stability and the antibacterial ability of AKD slaking speed, raising AKD emulsion, reduce sizing agent consumption and papermaking cost, this product is harmless to ecological environment, be easy to degraded at occurring in nature, can not increase paper and discongest difficulty, can replace or partly replace cationic starch and the poly-powder of gram.
The specific embodiment
The invention will be further described below by specific embodiment, but the present invention should not be subjected to the restriction of these embodiment.
Embodiment 1:
In the 10000L polymeric kettle, add deionized water 2501kg, methylallyl alcohol 12kg, regulate mixing speed to 250r/min.Take by weighing 65% dimethyl diallyl ammonium chloride 4808kg and go into head tank 1, take by weighing 2,2 '-azo (2-methyl-propyl amidine) dihydrochloride 7.02kg is dissolved in the 432.5kg deionized water and goes into head tank 2.The heated polymerizable still is warming up to 105 ℃, open two head tank bottom valves, drip toward polymeric kettle simultaneously, control head tank 1 dripped off on time at 60 minutes, head tank 2 was regulated a flow in per 20 minutes, and flow velocity is respectively: 130 liters/hour, 168 liters/hour, 224 liters/hour, 312 liters/hour, 455 liters/hour.Drip off the back constant 105 ℃ 60 minutes, add aluminum sulfate 150kg, stirred 30 minutes, be cooled to 50 ℃, adjusting pH to 6.0, packing stirs.
Embodiment 2:
In the 10000L polymeric kettle, add deionized water 2501kg, propenyl 10.5kg, regulate mixing speed to 250r/min.Take by weighing 65% dimethyl diallyl ammonium chloride 4808kg and go into head tank 1, take by weighing azo diisopropyl imidazoline salt hydrochlorate 5.13kg and be dissolved in the 432.5kg deionized water and go into head tank 2.The heated polymerizable still is warming up to 95 ℃, open two head tank bottom valves, drip toward polymeric kettle simultaneously, control head tank 1 dripped off on time at 20 minutes, head tank 2 was regulated a flow in per 20 minutes, and flow velocity is respectively: 130 liters/hour, 168 liters/hour, 224 liters/hour, 312 liters/hour, 455 liters/hour.Drip off the back constant 105 ℃ 60 minutes, add aluminum sulfate 230kg, stirred 30 minutes, be cooled to 50 ℃, adjusting pH to 6.0, packing stirs.
Embodiment 3:
In the 10000L polymeric kettle, add deionized water 1050kg, propenyl 8.3kg, regulate mixing speed to 250r/min.Take by weighing 60% dimethyl diallyl ammonium chloride 6510kg and go into head tank 1, take by weighing 2,2 '-azo (2-methyl-propyl amidine) dihydrochloride 30.71kg is dissolved in the 432.5kg deionized water and goes into head tank 2.The heated polymerizable still is warming up to 115 ℃, open two head tank bottom valves, drip toward polymeric kettle simultaneously, control head tank 1 dripped off on time at 30 minutes, head tank 2 was regulated a flow in per 20 minutes, and flow velocity is respectively: 130 liters/hour, 168 liters/hour, 224 liters/hour, 312 liters/hour, 455 liters/hour.Drip off the back constant 105 ℃ 60 minutes, add aluminum sulfate 160kg, stirred 30 minutes, be cooled to 50 ℃, adjusting pH to 6.0, packing stirs.
Embodiment 4:
In the 10000L polymeric kettle, add deionized water 1500kg, propenyl 11kg, regulate mixing speed to 250r/min.Take by weighing 62% dimethyl diallyl ammonium chloride 6300kg and go into head tank 1, take by weighing azo diisopropyl (N-3-propionyloxy) amidine hydrochloride 20.85kg and be dissolved in the 287kg deionized water and go into head tank 2.The heated polymerizable still is warming up to 110 ℃, open two head tank bottom valves, drip toward polymeric kettle simultaneously, control head tank 1 dripped off on time at 60 minutes, head tank 2 was regulated a flow in per 20 minutes, and flow velocity is respectively: 87 liters/hour, 112 liters/hour, 149 liters/hour, 208 liters/hour, 303 liters/hour.It is constant in 105 ℃, 60 minutes to drip off the back, adds aluminum sulfate 190kg, stirs 30 minutes, is cooled to 50 ℃, regulates pH to 6.0, and packing stirs.
Embodiment 5:
In the 10000L polymeric kettle, add deionized water 2960kg, propenyl 15kg, regulate mixing speed to 250r/min.Take by weighing 65% dimethyl diallyl ammonium chloride 6010kg and go into head tank 1, take by weighing azo diisopropyl imidazoline salt hydrochlorate 8.77kg and be dissolved in the 860kg deionized water and go into head tank 2.The heated polymerizable still is warming up to 105 ℃, open two head tank bottom valves, drip toward polymeric kettle simultaneously, control head tank 1 dripped off on time at 30 minutes, head tank 2 was regulated a flow in per 20 minutes, and flow velocity is respectively: 261 liters/hour, 336 liters/hour, 447 liters/hour, 624 liters/hour, 909 liters/hour.Drip off the back constant 105 ℃ 60 minutes, add aluminum sulfate 150kg, stirred 30 minutes, be cooled to 50 ℃, adjusting pH to 6.0, packing stirs.
Embodiment 6:
In the 10000L polymeric kettle, add deionized water 3360kg, methylallyl alcohol 18kg, regulate mixing speed to 250r/min.Take by weighing 65% dimethyl diallyl ammonium chloride 6010kg and go into head tank 1, take by weighing azo diimidazole quinoline base propane dithionate 9.45kg and be dissolved in the 432.5kg deionized water and go into head tank 2.The heated polymerizable still is warming up to 95 ℃, open two head tank bottom valves, drip toward polymeric kettle simultaneously, control head tank 1 dripped off on time at 60 minutes, head tank 2 was regulated a flow in per 20 minutes, and flow velocity is respectively: 130 liters/hour, 168 liters/hour, 224 liters/hour, 312 liters/hour, 455 liters/hour.Drip off the back constant 105 ℃ 60 minutes, add aluminum sulfate 120kg, stirred 30 minutes, be cooled to 50 ℃, adjusting pH to 6.0, packing stirs.
Claims (6)
1, the preparation method of cation AKD maturing promotor, it is characterized in that: in polyplant, add solvent orange 2 A and monomers B, stirring is warming up to 60-150 ℃ polymerization temperature, drip the aqueous solution and the initiator solution of dimethyl diallyl ammonium chloride simultaneously, dimethyl diallyl ammonium chloride is controlled at time t1 and at the uniform velocity drips off in 0-120 minute, initiator solution is controlled in 5 hours and drips off, it is constant in above-mentioned polymerization temperature 0-120 minute to drip off the back, add auxiliary agent C, stirred 10-120 minute, be cooled to below 10-80 ℃, regulating the pH value is 1.0-7.0, and stirring gets product.
Described solvent orange 2 A is at least a in the mixture of washings, water-miscible organic solvent and water after deionized water, running water, the preceding batch of production, and the quality sum of water is no less than 50% of the total amount that feeds intake in the solvent gross mass and the dimethyl diallyl ammonium chloride aqueous solution; Above-mentioned water-miscible organic solvent is meant the water-soluble organic compounds that contains aerobic or nitrogen element, and the quality of water-miscible organic solvent is not more than 5% of the total amount that feeds intake;
Described monomers B is selected from least a in the unsaturated fatty alcohol, and the percentage that the mole consumption of monomers B accounts for dimethyl diallyl ammonium chloride mole consumption is 0.001%-30%;
Dimethyl diallyl ammonium chloride content is at least 50% in the described dimethyl diallyl ammonium chloride aqueous solution, is not more than 75%;
Described initiator solution is the aqueous solution of azo-compound, and the initator mass content in the initiator solution is not more than 10%; The weight ratio of initator and dimethyl diallyl ammonium chloride is between 0.0001 to 0.1;
Described auxiliary agent C is the aqueous solution of inorganic salts, and the consumption of auxiliary agent C is controlled at the 0.01-10% of gained finished product total amount.
2, preparation method according to claim 1 is characterized in that: described polymerization temperature is 80-120 ℃.
3, preparation method according to claim 1, it is characterized in that: described azo-compound is selected from: azo diisopropyl imidazoline salt hydrochlorate, 2,2 '-azo (2-methyl-propyl amidine) dihydrochloride, 4, at least a in 4 '-azo (4-cyanopentanoic acid), azo diimidazole quinoline base propane dithionate, azo diisopropyl (N-3-propionyloxy) amidine hydrochloride, azo diisopropyl (N-ethoxy) imidazoline salt hydrochlorate, the azo diisopropyl imidazoline.
4, preparation method according to claim 1 is characterized in that: described time t1 is 0-60 minute.
5, preparation method according to claim 1 is characterized in that: the rate of addition of initiator solution changes in gradient, that is: rate of addition increases gradually, and the initator mole flow velocity after per 20 minutes increases 1.0-2.0 doubly.
6, preparation method according to claim 1 is characterized in that: described auxiliary agent C is selected from: the aqueous solution of aluminum sulfate, aluminium chloride, aluminium polychloride, auxiliary agent C consumption is controlled at the 1-5% of gained finished product total amount.
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| CN2008100231689A CN101324042B (en) | 2008-07-16 | 2008-07-16 | Preparation of cation AKD maturing promotor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088861A (en) * | 2015-08-13 | 2015-11-25 | 合肥龙发包装有限公司 | Emulsifier making AKD glue fast cured |
| CN105601783A (en) * | 2016-01-27 | 2016-05-25 | 广东省建筑材料研究院 | Preparing method for mud stopping agent used for compound polycarboxylate superplasticizer |
| CN106632846A (en) * | 2016-12-27 | 2017-05-10 | 山东源根化学技术研发有限公司 | AKD (Alkyl Ketene Dimer) reinforcement accelerator for surface glue and preparation method thereof |
-
2008
- 2008-07-16 CN CN2008100231689A patent/CN101324042B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088861A (en) * | 2015-08-13 | 2015-11-25 | 合肥龙发包装有限公司 | Emulsifier making AKD glue fast cured |
| CN105601783A (en) * | 2016-01-27 | 2016-05-25 | 广东省建筑材料研究院 | Preparing method for mud stopping agent used for compound polycarboxylate superplasticizer |
| CN105601783B (en) * | 2016-01-27 | 2018-06-22 | 广东省建筑材料研究院 | A kind of preparation method of compound polycarboxylate water-reducer resistance mud agent |
| CN106632846A (en) * | 2016-12-27 | 2017-05-10 | 山东源根化学技术研发有限公司 | AKD (Alkyl Ketene Dimer) reinforcement accelerator for surface glue and preparation method thereof |
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| CN101324042B (en) | 2011-02-09 |
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Effective date of registration: 20110216 Address after: 215613 Jiangsu city in Zhangjiagang Province town of Phoenix Phoenix Road No. 1 Jiangsu Fu Miao Polytron Technologies Inc Patentee after: Jiangsu Feymer Technology Co., Ltd. Address before: 215613 Fenghuang Town, Zhangjiagang, Jiangsu Patentee before: Feixiang Chemical Co., Ltd., Jiangsu |