CN105001410A - Novel positive ion fixative preparing method - Google Patents
Novel positive ion fixative preparing method Download PDFInfo
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- CN105001410A CN105001410A CN201510443641.9A CN201510443641A CN105001410A CN 105001410 A CN105001410 A CN 105001410A CN 201510443641 A CN201510443641 A CN 201510443641A CN 105001410 A CN105001410 A CN 105001410A
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- dimethylamine
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Abstract
The invention discloses a novel positive ion fixative preparing method. The novel positive ion fixative preparing method comprises the following steps that mixing is conducted by using dimethylamine as the main raw material, using hexamethylenediamine and dimethylamino-ethyl methylacrylate as auxiliary materials and using water as solvent, so that a mixed monomer is formed, wherein the molar ratio of the hexamethylendiamine to the dimethylamine is 0.01-0.5:1; epoxy chloropropane is dripped into the mixed monomer in the first step, so that a pre-polymerized monomer is formed, wherein the molar ratio of the epoxy chloropropane to the mixed monomer is 0.5-4:1, and the reaction temperature is controlled between 10 DEG C and 60 DEG C; after dripping is completed, the temperature is kept between 70 DEG C and 95 DEG C, and water is added and the reaction is ended when the viscosity is increased to 300-1000 cps; inorganic acid and water are added into an obtained product, and the pH value is adjusted to be 3-5. According to the novel positive ion fixative preparing method, the reaction condition is mild, the reaction yield is high, and sudden polymerization caused by direct polymerization is avoided; in addition, the electric charge density is higher than that of similar products in China and foreign counties by 10%, the production cost is low, and the method is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to and determine the preparation method of agent, particularly relate to a kind of preparation method using anion garbage capturing agent in papermaking.
Background technology
Determine agent and be commonly called as anion garbage capturing agent, English name anionic trash catcher is called for short ATC or fixative, be the polymkeric substance of the linear low molecule quality of a class Gaoyang electric density.
Since 20th century, paper industry is developed rapidly, the particularly change of papermaking material structure, make the aggregation extent of the interfering negatively charged ion of wet end of machine and concentration more and more higher, cause the copy paper system paper that breaks frequent, become paper to there will be paper defects, and uninterrupted working time is short, turnout reduces.Reduce the method for the anionic trash impact in papermaking systems, with anion garbage capturing agent, pre-treatment is carried out to slurry exactly.
Organic and the inorganic two large classes of anion garbage capturing agent, the people such as Brouwer have studied the impact of different anions trash catchers on colloidalmaterial and tiny component, and organic ATC effectively can reduce the cationic demand of fiber surface.The maximum advantage of organic ATC be not by the impact of pH on copy paper system also without affecting, and consumption is little, and effect is also clearly.
Determine agent usually to be formed by cationic monomer and epoxy chloropropane ring-opening polymerization, the lower general room temperature of activation energy that agent needs are determined in preparation just can be carried out, but finished product does not need too high molecular weight, the formation of crossing high molecular weight polymers causes product electric density low, lose the ability catching anionic trash, therefore in order to prevent reaction sudden and violent gathering from strictly will control reaction conditions.Determine agent in order to what obtain high charge density, people have carried out large quantifier elimination to the synthetic technology of determining agent, and the technical measures of employing mainly comprise following several large class.
One, control temperature of reaction, control the reaction times.Zhou Haijun as outstanding in Guo Wei reports and controls temperature of reaction and reaction times in " papermaking chemical product and application ".
Two, add organic amine, add the organic amine of two carbon atoms to six carbon atom as EP0431739A1 adopts.
Summary of the invention
The object of this invention is to provide a kind of novel cation and determine the preparation method of agent, the novel cation that this preparation method obtains determines the wider catching range such as double bond class of anionic trash and long-chain anionoid rubbish agent to have to(for) anionic trash, and reaction conditions is gentle, reaction yield is high, what avoid that direct polymerization causes is sudden and violent poly-, electric density is more than 400, and cheap, is suitable for dropping into large-scale industrial production.
To achieve the above object of the invention, the technical solution used in the present invention is: a kind of novel cation determines the preparation method of agent, comprises the following steps:
Step one, be body material by dimethylamine, hexanediamine and dimethylaminoethyl methacrylate are auxiliary material, water carries out being mixed to form mix monomer as solvent, described hexanediamine: dimethylamine mol ratio is 0.01 ~ 0.5:1, described dimethylaminoethyl methacrylate: dimethylamine mol ratio is 0.01 ~ 0.5:1;
Step 2, epoxy chloropropane is instilled step one mix monomer in formed pre-polymerization monomer (, and this epoxy chloropropane and mix monomer mol ratio are 0.5 ~ 4:1, and temperature of reaction controls at 10 ~ 60 DEG C, and time for adding controls at 1 ~ 3h;
After step 3, dropping terminate, be incubated to 70 ~ 95 DEG C, insulation 1 ~ 4h, treat that viscosity rises to 300 ~ 1000cps viscosity, add water termination reaction;
Step 4, to obtain in product in step 3 and add mineral acid and water regulates pH to 3 ~ 5, thus obtain positively charged ion and determine agent.
The technical scheme that technique scheme is improved further is as follows:
1. in such scheme, in described mix monomer, hexanediamine and dimethylamine mol ratio are 0.03 ~ 0.3:1, and the mol ratio of described dimethylaminoethyl methacrylate and dimethylamine is 0.02 ~ 0.4:1.
2., in such scheme, in described step 4, add 50% sulfuric acid modulation pH to 3 ~ 5.
3., in such scheme, described dimethylamine adopts mass concentration to be 40% dimethylamine agueous solution.
4., in such scheme, it is 49 ~ 51% that positively charged ion that described step 4 obtains determines agent solid content.
Due to the utilization of technique scheme, the present invention compared with prior art has following advantages:
Novel cation of the present invention determines the preparation method of agent, adopts and adds hexanediamine, effective introduces reactive group and diamine or polyamines, increases the chain length of polymkeric substance, can combine with the anionic trash in system better, add dimethylaminoethyl methacrylate, introduce double bond namely containing the monomer that double bond can be polymerized with epoxy chloropropane, can combine with the double bond in anionic part rubbish, it is sudden and violent poly-that this patent avoids that the direct polymerization of single dimethylamine and epoxy chloropropane causes, avoid too much macromolecular formation, crossing macromolecular formation causes product electric density low, lose the ability catching anionic trash, and take to control polymkeric substance viscosity, the higher charge density of product can be controlled preferably, product dilutes 10000 times and adopts BTG PCD-04 to measure, determining dilution agent 10000 times adopts BTG PCD-04 to carry out measuring its electric density 450, and it is cheap, be suitable for dropping into large-scale industrial production.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1: a kind of novel cation determines the preparation method of agent, comprises the following steps:
Step one, be body material by dimethylamine, hexanediamine and dimethylaminoethyl methacrylate are that auxiliary material mixes, and are specially: hexanediamine 15g, dimethylaminoethyl methacrylate 25.7g, dimethylamine (40%) aqueous solution 192.4g, water 50g mix;
Step 2, epoxy chloropropane 190 g;
Step 3, dropping temperature control at 20-30 DEG C, and time for adding controls at 1 ~ 3h;
Step 4, drip and terminate after, be warming up to 85 DEG C, insulation 2.5h, treat that viscosity rises to 300 ~ 700cps viscosity and to add water 100g termination reaction.
Step 5, add 50% sulfuric acid 10 g, 40g water adjusts pH to 3-5.
The present embodiment obtains finished product 610g through synthesis, pH4.5, solid content 50.8%, dilutes 10000 times and carries out measurement electric density 420 with BTG PCD-04.
Embodiment 2: a kind of novel cation determines the preparation method of agent, comprises the following steps:
Step one, be body material hexanediamine and dimethylaminoethyl methacrylate by dimethylamine be that auxiliary material mixes, hexanediamine 20g, dimethylaminoethyl methacrylate 12.8g, dimethylamine (40%) aqueous solution 180.5g, water 150g mixes;
Step 2, epoxy chloropropane 290 g;
Step 3, dropping temperature control at 40-50 DEG C, and time for adding controls at 1 ~ 3h;
Step 4, drip and terminate after, be warming up to 75 DEG C, insulation 4h, treat that viscosity rises to 300 ~ 700cps viscosity and to add water 100g termination reaction.
Step 5, add 50% sulfuric acid 15 g, 40g water adjusts pH to 3-5.
The present embodiment obtains finished product 790g through synthesis, pH 3.5, solid content 50.2%, dilutes 10000 times of electric density 410.
Embodiment 3: a kind of novel cation determines the preparation method of agent, comprises the following steps:
Step one, be body material hexanediamine and dimethylaminoethyl methacrylate by dimethylamine be that auxiliary material mixes, hexanediamine 25g, dimethylaminoethyl methacrylate 38.5g, dimethylamine (40%) aqueous solution 170g, water 100g mixes;
Step 2, epoxy chloropropane 236.5 g;
Step 3, dropping temperature control at 30-40 DEG C, and time for adding controls at 1 ~ 3h;
Step 4, drip and terminate after, be warming up to 90 DEG C, insulation 2h, treat that viscosity rises to 300 ~ 700cps viscosity and to add water 100g termination reaction.
Step 5, add 50% sulfuric acid 20g, 40g water adjusts pH to 3-5.
The present embodiment obtains finished product 715g through synthesis, pH3.6, solid content 49.9%, dilutes 10000 times of electric density 450.
According to embodiment 1,2 and 3, the product electric density that mutual comparative example 3 obtains is the highest, because embodiment 3 hexanediamine, the ratio that dimethylaminoethyl methacrylate accounts for mix monomer is the highest, the ratio of epoxy chloropropane and mix monomer is the highest, be conducive to the formation of high charge density, the moderate reaction of synthesis temperature is gentleer, and these conditions are all conducive to the formation of high charge density.
Comparative example 1: a kind of preparation method determining agent, comprises the following steps:
Step one, be body material by dimethylamine, dimethylamine (40%) aqueous solution 192.4, water 50g 10g monomer (as following table 1), mixes;
Step 2, epoxy chloropropane 190 g;
Step 3, dropping temperature control at 20-30 DEG C;
After step 4, dropping terminate, be warming up to 85 DEG C, insulation 1h, treats that viscosity rises to 300 ~ 700cps viscosity and adds 100g water termination reaction;
Step 5, add 50% sulfuric acid 10g, 20g water adjusts pH to 3-5.
Table 1: difference adds the impact of monomer on product electric density
Table 1
| Sequence number | Hexanediamine | Diethylenetriamine | Dimethylaminoethyl methacrylate | Dimethylaminoethyl methyl esters | Quality product/g | Yield/% | Electric density |
| 1 | 15 | / | / | / | 545 | 96.9% | 350 |
| 2 | / | 15 | / | / | 549 | 97.6% | 260 |
| 3 | / | / | 15 | / | 550 | 97.8% | 340 |
| 4 | / | / | / | 15 | 548 | 97.4% | 270 |
Table 1 illustrate adding of hexanediamine and the product yield that dimethylaminoethyl methacrylate obtains higher, electric density is higher.
Comparative example 2: a kind of preparation method determining agent, comprises the following steps:
Step one, be raw material by dimethylamine, dimethylamine (40%) aqueous solution 192.4g, water 50g mixes;
Step 2, epoxy chloropropane 190 g
Step 3, dropping temperature control at 40-50 DEG C;
Step 4, drip and terminate after, be warming up to 75 DEG C, insulation 4h, treat that viscosity rises to 300 ~ 700cps viscosity and to add water 100g termination reaction.
Step 5, add 50% sulfuric acid 10 g, adjust pH to 3-5.
The present embodiment obtains finished product 525 g through synthesis, pH 3.5, solid content 49.8%, dilutes 10000 times of electric density 240.
Comparative example 1, adds monomer methacrylic dimethylamino methyl esters in mix monomer, methacrylic dimethylamino methyl esters is not so good as the reactive behavior of dimethylaminoethyl methacrylate and epoxy chloropropane, and thus electric density is low; Add monomer diethylenetriamine in mix monomer, the electronics that diethylenetriamine provides is not so good as hexanediamine, so electric density is low.Comparative example 2, single dimethylamine and epoxy chloropropane electric density low, reaction finished product there is a small amount of bits and sudden and violent polymers through filtration.
Hexanediamine and dimethylamine mol ratio low lower than 0.03:1 electric density, hexanediamine and dimethylamine mol ratio be greater than 0.3:1 reaction more wayward; The mol ratio of dimethylaminoethyl methacrylate and dimethylamine is low lower than 0.02:1 electric density, and the mol ratio of dimethylaminoethyl methacrylate and dimethylamine is greater than the quality guaranteed period that 0.4:1 affects product
Above-described embodiment, only for technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.
All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (5)
1. novel cation determines a preparation method for agent, it is characterized in that: comprise the following steps:
Step one, be body material by dimethylamine, hexanediamine and dimethylaminoethyl methacrylate are auxiliary material, water carries out being mixed to form mix monomer as solvent, described hexanediamine: dimethylamine mol ratio is 0.01 ~ 0.5:1, described dimethylaminoethyl methacrylate: dimethylamine mol ratio is 0.01 ~ 0.5:1;
Step 2, epoxy chloropropane is instilled step one mix monomer in form pre-polymerization monomer, and the mol ratio of the mixture of this epoxy chloropropane and dimethylamine, hexanediamine, dimethylaminoethyl methacrylate is 0.5 ~ 4:1, temperature of reaction controls at 10 ~ 60 DEG C, and time for adding controls at 1 ~ 3h;
After step 3, dropping terminate, be incubated to 70 ~ 95 DEG C, insulation 1 ~ 4h, treat that viscosity rises to 300 ~ 1000cps viscosity, add water termination reaction;
Step 4, to obtain in product in step 3 and add mineral acid and water regulates pH to 3 ~ 5, thus obtain positively charged ion and determine agent.
2. novel cation according to claim 1 determines the preparation method of agent, it is characterized in that: in described mix monomer, hexanediamine and dimethylamine mol ratio are 0.03 ~ 0.3:1, the mol ratio of described dimethylaminoethyl methacrylate and dimethylamine is 0.02 ~ 0.4:1.
3. novel cation according to claim 1 determines the preparation method of agent, it is characterized in that: add 50% sulfuric acid modulation pH to 3 ~ 5 in described step 4.
4. novel cation according to claim 1 determines the preparation method of agent, it is characterized in that: described dimethylamine adopts mass concentration to be 40% dimethylamine agueous solution.
5. novel cation according to claim 1 determines the preparation method of agent, it is characterized in that: it is 49 ~ 51% that positively charged ion that described step 4 obtains determines agent solid content.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114150527A (en) * | 2021-12-17 | 2022-03-08 | 杭州绿邦科技有限公司 | Retention and drainage aid |
| CN114164702A (en) * | 2021-12-17 | 2022-03-11 | 杭州绿邦科技有限公司 | Processing method of cation fixative |
| CN114250646A (en) * | 2021-12-08 | 2022-03-29 | 杭州市化工研究院有限公司 | Preparation method of special anion garbage catching agent for fruit cultivation bag paper |
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| CN102558552A (en) * | 2011-12-10 | 2012-07-11 | 江阴市尼美达助剂有限公司 | Preparation method of formaldehyde-free color fixative |
| CN103981752A (en) * | 2014-04-29 | 2014-08-13 | 华南理工大学 | Preparation method for cationic modified fixer applied to DCS (Dissolved and Colloidal Substances) |
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Patent Citations (3)
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| WO2003016986A1 (en) * | 2001-08-16 | 2003-02-27 | Toray Industries, Inc. | Colored hydrous contact lens and method for preparation thereof |
| CN102558552A (en) * | 2011-12-10 | 2012-07-11 | 江阴市尼美达助剂有限公司 | Preparation method of formaldehyde-free color fixative |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250646A (en) * | 2021-12-08 | 2022-03-29 | 杭州市化工研究院有限公司 | Preparation method of special anion garbage catching agent for fruit cultivation bag paper |
| CN114150527A (en) * | 2021-12-17 | 2022-03-08 | 杭州绿邦科技有限公司 | Retention and drainage aid |
| CN114164702A (en) * | 2021-12-17 | 2022-03-11 | 杭州绿邦科技有限公司 | Processing method of cation fixative |
| CN114164702B (en) * | 2021-12-17 | 2023-02-14 | 杭州绿邦科技有限公司 | Processing method of cation fixative |
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