CN105386367A - Preparation method of wet strength agent for papermaking - Google Patents
Preparation method of wet strength agent for papermaking Download PDFInfo
- Publication number
- CN105386367A CN105386367A CN201510910583.6A CN201510910583A CN105386367A CN 105386367 A CN105386367 A CN 105386367A CN 201510910583 A CN201510910583 A CN 201510910583A CN 105386367 A CN105386367 A CN 105386367A
- Authority
- CN
- China
- Prior art keywords
- wet strength
- strength agent
- preparation
- paper making
- acid
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/18—Reinforcing agents
- D21H21/20—Wet strength agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/48—Polymers modified by chemical after-treatment
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/55—Polyamides; Polyaminoamides; Polyester-amides
Abstract
The invention relates to the technical field of papermaking additive, and specifically relates to a preparation method of a wet strength agent for papermaking. The preparation method comprises the following steps: step one, under the protection of nitrogen gas, mixing and stirring polycarboxylic acid and polyamine, then adding a catalyst, carrying out reactions for 2 to 4 hours at a temperature of 90 to 130 DEG C, and cooling to obtain a polyamide polyamine prepolymer; step two, adding dimer acid into the polyamide polyamine prepolymer obtained in the step one, and carrying out reactions for 5 to 9 hours at a temperature of 160 to 180 DEG C to obtain a wet strength agent intermediate; step three, adding water into the wet strength agent intermediate obtained in the step two to obtain a wet strength agent intermediate solution, then adding a cationic etherifying agent, evenly stirring, slowly adding epoxy chloropropane, heating the system to a temperature of 50 to 70 DEG C, and carrying out reactions for 2 to 4 hours; step four, adjusting the pH value of the reaction system to 2-3 to obtain the wet strength agent. The prepared wet strength agent can well improve the wet strength of paper, and moreover, the retention rate is high.
Description
Technical field
The present invention relates to paper making additive technical field, relate more specifically to a kind of preparation method of wet strength agent for paper making.
Background technology
Polyamide-Polyamsne-Epichlorohydrin resin (being called for short PPE) is a kind of heat curing-type water-soluble resin, and it is good that it has into paper wet strength, and retention is high, consumption is few, nontoxic and not release formaldehyde, being applicable to the advantages such as neutral and alkali copy paper, is a class wet strength agent for papermaking of present paper industry extensive use.
At present, PPE wet strength agent for papermaking generates polyamide polyamine primarily of adipic acid and diethylenetriamine under the effect of catalyst, then obtains with epichlorohydrin reaction.Because PPE resin is the very highly active macromolecular resin of one, easily there is intramolecular crosslinking in its solid content height, its product is easy to gel, so PPE wet strength agent solid content is low, generally about 12.5%, causes product utilization rate to reduce, and cost of transportation increases; On the other hand, PPE resin is a kind of thermosetting resin, and needing could slaking completely in certain temperature and regular hour, produces complete wet strength effect.The curing time of conventional P PE wet strength agent is long, and paper once paper machine can only produce the wet strength effect of about 50%, generally at room temperature will deposit and a week more than could produce wet strength effect completely, can affect the use of paper.
Summary of the invention
The present invention, for overcoming at least one defect described in above-mentioned prior art, provides a kind of preparation method of wet strength agent for paper making.Present invention process is simple, easy to operate, and the wet strength agent that the method obtains can be good at the wet strength improving paper, and retention is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of wet strength agent for paper making, wherein, comprises the following steps:
S1. under nitrogen protection, first polycarboxylic acids and polyamine are uniformly mixed, then add catalyst, at temperature 90-130 DEG C, reaction 2-4h, finally lowers the temperature, obtains polyamide polyamines prepolymer;
S2. joined by dimeric dibasic acid in the polyamide polyamines prepolymer that step S1 obtains, at 160-180 DEG C, reaction 5-9h, obtains wet strength agent intermediate;
S3. at room temperature, thin up in the wet strength agent intermediate that step S2 obtains, obtains wet strength agent midbody solution, then adds cationic etherifying agent, after stirring, slowly add epoxychloropropane, be warming up to 50-70 DEG C, reaction 2-4h;
S4. regulate pH value to 2-3 of reaction system, obtain described wet strength agent.
Preferably, in described step S1, polycarboxylic acids is the copolymer of acrylic acid, methacrylic acid, maleic acid, maleic anhydride, cinnamic acid.
Preferably, in described step S1, polyamine is one or more in ethylenediamine, butanediamine, triethylamine, diethylenetriamine.
Preferably, in described step S1, catalyst is sulfuric acid or phosphoric acid, and the consumption of described catalyst is 1%-4% of polyamine weight.
Preferably, in described step S1, the weight ratio of described polycarboxylic acids and polyamine is 0.6-0.8:1.
Preferably, in described step S2, the weight ratio of described dimeric dibasic acid and polycarboxylic acids is 1:0.18-0.25.
Preferably, in described step S3, the weight ratio of described cationic etherifying agent, epoxychloropropane and wet strength agent intermediate is 0.06-0.095:0.16-0.19:1.
Compared with the existing technology, beneficial effect of the present invention is:
Present invention process is simple, easy to operate, and the wet strength agent that the method obtains can be good at the wet strength improving paper, and retention is high.Wet strength agent reaction temperature prepared by the present invention and, stablize controlled, product not easily overreact and gel, solid content is higher; And the ammonium cation based compound solidification temperature obtained is lower, adds easier slaking after in paper to, easy to use, and cost is low.
Detailed description of the invention
Embodiment 1
In four-hole boiling flask, under logical nitrogen protection, first 45 grams of diethylenetriamines and 30 grams of acrylic acid are uniformly mixed; Add 0.45 gram of 50% sulfuric acid afterwards, at temperature 90 DEG C, react 2 hours; Finally lower the temperature, obtain polyamide polyamine prepolymer.
In the prepolymer of above-mentioned gained, add dimeric dibasic acid 160 grams, be warming up to 160 DEG C, insulation reaction 5 hours, obtains wet strength agent intermediate.
At room temperature, in the intermediate of above-mentioned gained, first add 300 grams of dilution waters, then add 15 grams of 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, after stirring, slowly add 40 grams of epoxychloropropane, after adding, be warming up to 50 DEG C, insulation reaction 2 hours.Finally add sulfuric acid adjust ph to 2, be diluted with water to the wet strength agent for papermaking that solid content is 25%.
Embodiment 2
In four-hole boiling flask, under logical nitrogen protection, first 50 grams of diethylenetriamines and 35 grams of acrylic acid are uniformly mixed; Add 1.25 gram of 50% sulfuric acid afterwards, at temperature 110 DEG C, react 3 hours; Finally lower the temperature, obtain polyamide polyamine prepolymer.
In the prepolymer of above-mentioned gained, add dimeric dibasic acid 165 grams, be warming up to 170 DEG C, insulation reaction 7 hours, obtains wet strength agent intermediate.
At room temperature, in the intermediate of above-mentioned gained, first add 350 grams of dilution waters, then add 20 grams of 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, after stirring, slowly add 45 grams of epoxychloropropane, after adding, be warming up to 60 DEG C, insulation reaction 3 hours.Finally add sulfuric acid adjust ph to 2.5, be diluted with water to the wet strength agent for papermaking that solid content is 30%.
Embodiment 3
In four-hole boiling flask, under logical nitrogen protection, first 55 grams of diethylenetriamines and 40 grams of acrylic acid are uniformly mixed; Add 2.2 gram of 50% sulfuric acid afterwards, at temperature 130 DEG C, react 4 hours; Finally lower the temperature, obtain polyamide polyamine prepolymer.
In the prepolymer of above-mentioned gained, add dimeric dibasic acid 170 grams, be warming up to 180 DEG C, insulation reaction 9 hours, obtains wet strength agent intermediate.
At room temperature, in the intermediate of above-mentioned gained, first add 400 grams of dilution waters, then add 25 grams of 3-chloro-2-hydroxypropyl-trimethyl ammonium chlorides, after stirring, slowly add 50 grams of epoxychloropropane, after adding, be warming up to 70 DEG C, insulation reaction 4 hours.Finally add sulfuric acid adjust ph to 3, be diluted with water to the wet strength agent for papermaking that solid content is 35%.
Obviously, the above embodiment of the present invention is only used to example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.All any amendments done within the spirit and principles in the present invention, equivalent to replace and improvement etc., within the protection domain that all should be included in the claims in the present invention.
Claims (7)
1. a preparation method for wet strength agent for paper making, is characterized in that, comprises the following steps:
S1. under nitrogen protection, first polycarboxylic acids and polyamine are uniformly mixed, then add catalyst, at temperature 90-130 DEG C, reaction 2-4h, finally lowers the temperature, obtains polyamide polyamines prepolymer;
S2. joined by dimeric dibasic acid in the polyamide polyamines prepolymer that step S1 obtains, at 160-180 DEG C, reaction 5-9h, obtains wet strength agent intermediate;
S3. at room temperature, thin up in the wet strength agent intermediate that step S2 obtains, obtains wet strength agent midbody solution, then adds cationic etherifying agent, after stirring, slowly add epoxychloropropane, be warming up to 50-70 DEG C, reaction 2-4h;
S4. regulate pH value to 2-3 of reaction system, obtain described wet strength agent.
2. the preparation method of a kind of wet strength agent for paper making according to claim 1, is characterized in that, in described step S1, polycarboxylic acids is the copolymer of acrylic acid, methacrylic acid, maleic acid, maleic anhydride, cinnamic acid.
3. the preparation method of a kind of wet strength agent for paper making according to claim 1, is characterized in that, in described step S1, polyamine is one or more in ethylenediamine, butanediamine, triethylamine, diethylenetriamine.
4. the preparation method of a kind of wet strength agent for paper making according to claim 1, is characterized in that, in described step S1, catalyst is sulfuric acid or phosphoric acid, and the consumption of described catalyst is 1%-4% of polyamine weight.
5. the preparation method of a kind of wet strength agent for paper making according to claim 1, is characterized in that, in described step S1, the weight ratio of described polycarboxylic acids and polyamine is 0.6-0.8:1.
6. the preparation method of a kind of wet strength agent for paper making according to claim 1, is characterized in that, in described step S2, the weight ratio of described dimeric dibasic acid and polycarboxylic acids is 1:0.18-0.25.
7. the preparation method of a kind of wet strength agent for paper making according to claim 1, is characterized in that, in described step S3, the weight ratio of described cationic etherifying agent, epoxychloropropane and wet strength agent intermediate is 0.06-0.095:0.16-0.19:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510910583.6A CN105386367A (en) | 2015-12-10 | 2015-12-10 | Preparation method of wet strength agent for papermaking |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510910583.6A CN105386367A (en) | 2015-12-10 | 2015-12-10 | Preparation method of wet strength agent for papermaking |
Publications (1)
| Publication Number | Publication Date |
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| CN105386367A true CN105386367A (en) | 2016-03-09 |
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Family Applications (1)
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| CN201510910583.6A Pending CN105386367A (en) | 2015-12-10 | 2015-12-10 | Preparation method of wet strength agent for papermaking |
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| CN (1) | CN105386367A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108716161A (en) * | 2018-06-07 | 2018-10-30 | 华东理工大学 | A kind of preparation method of wet strength agent |
| CN109369909A (en) * | 2018-12-08 | 2019-02-22 | 浙江百斯特化工有限公司 | A kind of cation wet strength agent and preparation method thereof |
| CN109763380A (en) * | 2019-01-02 | 2019-05-17 | 江苏富淼科技股份有限公司 | A kind of wet strength agent for paper making and preparation method thereof |
| CN113293639A (en) * | 2021-05-11 | 2021-08-24 | 济宁南天农科化工有限公司 | Modified crosslinked polyamide polyamine cylinder sticking agent applicable to high temperature and preparation method thereof |
| CN113981735A (en) * | 2021-10-20 | 2022-01-28 | 广东省造纸研究所有限公司 | Preparation method of environment-friendly wet strength agent |
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| CN1966855A (en) * | 2006-10-19 | 2007-05-23 | 上海东升新材料有限公司 | Epoxy polyurethane resin wet-strengthening agent and method for preparing same |
| CN104710579A (en) * | 2015-03-19 | 2015-06-17 | 九洲生物技术（苏州）有限公司 | Wet strength agent, and preparation method and application of wet strength agent |
| CN105085906A (en) * | 2015-08-17 | 2015-11-25 | 广东省造纸研究所 | Preparation method of papermaking wet strength agent |
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2015
- 2015-12-10 CN CN201510910583.6A patent/CN105386367A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1966855A (en) * | 2006-10-19 | 2007-05-23 | 上海东升新材料有限公司 | Epoxy polyurethane resin wet-strengthening agent and method for preparing same |
| CN104710579A (en) * | 2015-03-19 | 2015-06-17 | 九洲生物技术（苏州）有限公司 | Wet strength agent, and preparation method and application of wet strength agent |
| CN105085906A (en) * | 2015-08-17 | 2015-11-25 | 广东省造纸研究所 | Preparation method of papermaking wet strength agent |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108716161A (en) * | 2018-06-07 | 2018-10-30 | 华东理工大学 | A kind of preparation method of wet strength agent |
| CN109369909A (en) * | 2018-12-08 | 2019-02-22 | 浙江百斯特化工有限公司 | A kind of cation wet strength agent and preparation method thereof |
| CN109763380A (en) * | 2019-01-02 | 2019-05-17 | 江苏富淼科技股份有限公司 | A kind of wet strength agent for paper making and preparation method thereof |
| CN109763380B (en) * | 2019-01-02 | 2021-12-21 | 江苏富淼科技股份有限公司 | Wet strength agent for papermaking and preparation method thereof |
| CN113293639A (en) * | 2021-05-11 | 2021-08-24 | 济宁南天农科化工有限公司 | Modified crosslinked polyamide polyamine cylinder sticking agent applicable to high temperature and preparation method thereof |
| CN113981735A (en) * | 2021-10-20 | 2022-01-28 | 广东省造纸研究所有限公司 | Preparation method of environment-friendly wet strength agent |
| CN113981735B (en) * | 2021-10-20 | 2022-05-31 | 广东省造纸研究所有限公司 | Preparation method of environment-friendly wet strength agent |
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Application publication date: 20160309 |
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