CN103806337A - Papermaking wet strengthening agent preparation method - Google Patents
Papermaking wet strengthening agent preparation method Download PDFInfo
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- CN103806337A CN103806337A CN201210445339.3A CN201210445339A CN103806337A CN 103806337 A CN103806337 A CN 103806337A CN 201210445339 A CN201210445339 A CN 201210445339A CN 103806337 A CN103806337 A CN 103806337A
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Abstract
The present invention relates to a papermaking wet strengthening agent preparation method, and belongs to the field of pulping papermaking. The papermaking wet strengthening agent preparation method comprises: dissolving diethylenetriamine in water to prepare a solution with a mass percent concentration of 30%; adding adipic acid to the solution, wherein the temperature of the solution is automatically increased at this time, water volatilizes along with the temperature increase, and the solution temperature can achieve 110-120 DEG C; adding a modifier M to the obtained solution, and continuously heating under stirring to achieve a temperature of 140-180 DEG C; and finally slowly adding water to the solution so as to cool the solution to achieve a temperature of 70 DEG C to produce an intermediate polyamide polyamine, continuously adding epichlorohydrin to the intermediate solution, carrying out a reaction for about 2 h, maintaining the pH value of the reaction system at 7.5-8.5, and stopping the reaction to obtain the wet strengthening agent. The prepared modified PAE wet strengthening agent can be directly added to the pulp, provides a better enhancing effect compared with other enhancing agents, and has characteristics of low price, wastewater pollution reduction, and weakening of corrosion on papermaking equipment.
Description
Technical field
The invention belongs to pulping and paper-making field, be specifically related to a kind of wet strength agent for papermaking collocation method.
Background technology
Cationic polyamide-epichlorohydrin resin (PAE) is wet strength agent the most frequently used in paper, and it has the features such as efficient, applied widely.PAE, except increasing the wet epistasis energy of paper, also can increase to some extent dry strength, and can be used as the retention agents of filler in paper-making process, improves the filter aid of paper output etc.But PAE price is higher, cost falls in order to save in factory, is finding the substitute of PAE always, makes paper product strength decreased, loses more than gain.Meanwhile, PAE paper-making pollution is larger, is unfavorable for the protection of environment.
Summary of the invention
Goal of the invention: for the deficiencies in the prior art, the object of this invention is to provide a kind of wet strength agent for papermaking and collocation method thereof, fallen cost in the same time that guarantees paper product intensity, and this method can alleviate contaminated wastewater, weaken the corrosion to paper making equipment.
Technical scheme: in order to realize foregoing invention object, the technical solution used in the present invention is as follows:
A kind of wet strength agent for papermaking collocation method, comprise the following steps: be first 30% solution by the water-soluble diethylenetriamine mass percentage concentration that is made into, then in described solution, add adipic acid, the now temperature automatic-ascending of described solution, moisture volatilizees thereupon, the temperature of described solution can reach 110-120 ℃, and then adds modifier M in described solution, under agitation continues to be heated to 140-180 ℃; In the most backward described solution, slowly add water, make described solution be cooled to 70 ℃, generate intermediate polyamide polyamine, in described midbody solution, continue to add epoxychloropropane, react about 2h, keeping pH value of reaction system is that 7.5-8.5 cessation reaction obtain wet strength agent.
The mass ratio of described adipic acid and diethylenetriamine and modifier M is 7:4:2.
The mol ratio of described polyamide polyamine and epoxychloropropane is between 1:1.4-1.8.
The wet strength agent outward appearance of telling is faint yellow thick liquid, and solid content is 12.5%, viscosity 0.03-0.1Pa.s.
In this invention, obtain PAE intermediate with adipic acid, diethylenetriamine and modifier M reaction, after being oxidized with epoxychloropropane, obtain wet strength agent; In the time changing the proportioning of adipic acid and diethylenetriamine and modifier M, viscosity to the intermediate polyamide polyamine generating is very large, this is because the viscosity of polyamide polyamine is relevant with its degree of polymerization, viscosity is large, and the degree of polymerization is large relatively, retention performance is good, so will rationally control the mass ratio of adipic acid, diethylenetriamine and modifier M in preparation process, optimum ratio is that the mass ratio of adipic acid and diethylenetriamine and modifier M is 7:4:2; On imido grpup, nitrogen easily and epoxychloropropane generation nucleophilic substitution, form cationic polyamide polymeric amine epichlorohydrin, it is as alkali slaking resin, under alkali condition, can form very soon cross-linked structure, in course of reaction, the variation of the mol ratio between polyamide polyester and epoxychloropropane is very large to the performance impact of polyamide polyamine, preferably determines that by experiment mol ratio between polyamide polyamine and epoxychloropropane is between 1:1.4-1.8.Adopting the modified product outward appearance that above method makes is faint yellow thick liquid, solid content 12.5%, viscosity 0.03-0.1Pa.s, water-soluble (1:10 dilution), without layering without precipitation, room temperature not stratified not gel half a year, pH value 4-5, room temperature is placed the half a year of gel not above.
Beneficial effect: for the deficiency of existing invention, the Modified PAE Resin Wet-strength Agent that the present invention makes can directly be added in slurry, strengthens effect and is better than other reinforcing agent, and cheap, can alleviate contaminated wastewater, weakens the corrosion to paper making equipment.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate the present invention, the present invention implements under take technical solution of the present invention as prerequisite, should understand these embodiment and only be not used in and limit the scope of the invention for the present invention is described.
In order to determine best preparation scheme, pH is 7, carries out handsheet test by reed pulp, and measures the wet strength of page, in carrying out blank test, has also measured the enhancing effect of the production piece that current factory generally applies in contrast, and result of the test is in table 1 and table 2.
Blank embodiment
In the experiment of table 2 empty, distilled water is added in reed pulp, addition accounts for 0.5% of reed pulp over dry quality, carries out handsheet experiment.Acquired results is in table 2.
Embodiment 1
In 1# experiment in table 1, first, by water-soluble diethylenetriamine 30% solution that is made into, then add adipic acid, now temperature automatic-ascending, moisture volatilizees thereupon, and temperature can reach 110-120 ℃, then adds modifier M, under agitation continues to be heated to 140-180 ℃.Reaction certain hour can stop heating.Slowly add water, be cooled to 70 ℃, in above-mentioned intermediate, add epoxychloropropane, react about 2h, maintenance system pH is 7.5-8.5, in the time that viscosity reaches requirement, adds immediately salt acid for adjusting pH value cessation reaction.In 1#, the mass ratio of adipic acid and diethylenetriamine and modifier M is 7:6:2.Mol ratio between polyamide polyamine and epoxychloropropane is 1:1.4.
In 1# experiment in table 2, adopt the prepared Modified PAE Resin Wet-strength Agent of 1# in table 1, solid content is 12.5%, and the water-soluble 1:10 that is diluted to, adds PAE wet strength agent in reed pulp, and addition accounts for 0.5% of reed pulp over dry quality, carries out handsheet experiment.Acquired results is in table 2.
Embodiment 2
In 2# experiment in table 1, first, by water-soluble diethylenetriamine 30% solution that is made into, then add adipic acid, now temperature automatic-ascending, moisture volatilizees thereupon, and temperature can reach 110-120 ℃, then adds modifier M, under agitation continues to be heated to 140-180 ℃.Reaction certain hour can stop heating.Slowly add water, be cooled to 70 ℃, in above-mentioned intermediate, add epoxychloropropane, react about 2h, maintenance system pH is 7.5-8.5, in the time that viscosity reaches requirement, adds immediately salt acid for adjusting pH value cessation reaction.In 1#, the mass ratio of adipic acid and diethylenetriamine and modifier M is 7:5:2.Mol ratio between polyamide polyamine and epoxychloropropane is 1:1.4.
In 2# experiment in table 2, adopt the prepared Modified PAE Resin Wet-strength Agent of 1# in table 1, solid content is 12.5%, and the water-soluble 1:10 that is diluted to, adds PAE wet strength agent in reed pulp, and addition accounts for 0.5% of reed pulp over dry quality, carries out handsheet experiment.Acquired results is in table 2.
Embodiment 3
In 3# experiment in table 1, first, by water-soluble diethylenetriamine 30% solution that is made into, then add adipic acid, now temperature automatic-ascending, moisture volatilizees thereupon, and temperature can reach 110-120 ℃, then adds modifier M, under agitation continues to be heated to 140-180 ℃.Reaction certain hour can stop heating.Slowly add water, be cooled to 70 ℃, in above-mentioned intermediate, add epoxychloropropane, react about 2h, maintenance system pH is 7.5-8.5, in the time that viscosity reaches requirement, adds immediately salt acid for adjusting pH value cessation reaction.In 1#, the mass ratio of adipic acid and diethylenetriamine and modifier M is 7:4:2.Mol ratio between polyamide polyamine and epoxychloropropane is 1:1.4.
In 3# experiment in table 2, adopt the prepared Modified PAE Resin Wet-strength Agent of 1# in table 1, solid content is 12.5%, and the water-soluble 1:10 that is diluted to, adds PAE wet strength agent in reed pulp, and addition accounts for 0.5% of reed pulp over dry quality, carries out handsheet experiment.Acquired results is in table 2.
Embodiment 4
In 4# experiment in table 1, first, by water-soluble diethylenetriamine 30% solution that is made into, then add adipic acid, now temperature automatic-ascending, moisture volatilizees thereupon, and temperature can reach 110-120 ℃, then adds modifier M, under agitation continues to be heated to 140-180 ℃.Reaction certain hour can stop heating.Slowly add water, be cooled to 70 ℃, in above-mentioned intermediate, add epoxychloropropane, react about 2h, maintenance system pH is 7.5-8.5, in the time that viscosity reaches requirement, adds immediately salt acid for adjusting pH value cessation reaction.In 1#, the mass ratio of adipic acid and diethylenetriamine and modifier M is 7:3:2.Mol ratio between polyamide polyamine and epoxychloropropane is 1:1.4.
In 4# experiment in table 2, adopt the prepared Modified PAE Resin Wet-strength Agent of 1# in table 1, solid content is 12.5%, and the water-soluble 1:10 that is diluted to, adds PAE wet strength agent in reed pulp, and addition accounts for 0.5% of reed pulp over dry quality, carries out handsheet experiment.Acquired results is in table 2.
Embodiment 5
In industrial goods experiment in table 2, adopt industry sampling wet strength agent, solid content is 12.5%, and the water-soluble 1:10 that is diluted to, adds this wet strength agent in reed pulp, and addition accounts for 0.5% of reed pulp over dry quality, carries out handsheet experiment.Acquired results is in table 2.
As shown in Table 1, the mass ratio of adipic acid and diethylenetriamine and modifier M is preferably 7:4:2.
As shown in Table 2, under the identical condition of other conditions, 1# is very large to reed pulp wet strength influence degree difference to 4# resin, and 3# scheme is preferred plan, and in the time that addition is 0.5%, wet strength is 28.05%, higher than 25.70% of general industry product.Note: table 1 result is measurement data in 50% solution of polyamide polyamine at 25 ℃.
The impact of table 1 raw material proportioning on polyamide polyamine viscosity
The impact of table 2 different resins on reed pulp paper wet strength
Claims (4)
1. a wet strength agent for papermaking collocation method, it is characterized in that: comprise the following steps: be first 30% solution by the water-soluble diethylenetriamine mass percentage concentration that is made into, then in described solution, add adipic acid, the now temperature automatic-ascending of described solution, moisture volatilizees thereupon, the temperature of described solution can reach 110-120 ℃, and then adds modifier M in described solution, under agitation continues to be heated to 140-180 ℃; In the most backward described solution, slowly add water, make described solution be cooled to 70 ℃, generate intermediate polyamide polyamine, in described midbody solution, continue to add epoxychloropropane, react about 2h, keeping pH value of reaction system is that 7.5-8.5 cessation reaction obtain wet strength agent.
2. wet strength agent for papermaking collocation method according to claim 1, is characterized in that: the mass ratio of described adipic acid and diethylenetriamine and modifier M is 7:4:2.
3. wet strength agent for papermaking collocation method according to claim 1, is characterized in that: the mol ratio of described polyamide polyamine and epoxychloropropane is between 1:1.4-1.8.
4. wet strength agent for papermaking collocation method according to claim 1, is characterized in that: the wet strength agent outward appearance of telling is faint yellow thick liquid, solid content is 12.5%, viscosity 0.03-0.1Pa.s.
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| CN201210445339.3A CN103806337A (en) | 2012-11-09 | 2012-11-09 | Papermaking wet strengthening agent preparation method |
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| CN201210445339.3A CN103806337A (en) | 2012-11-09 | 2012-11-09 | Papermaking wet strengthening agent preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017207A (en) * | 2014-06-12 | 2014-09-03 | 上海东升新材料有限公司 | Paper making/breaking control agent and preparation method thereof |
| CN109208382A (en) * | 2018-11-07 | 2019-01-15 | 济宁明升新材料有限公司 | A kind of wet strengthening agents for papermaking and preparation method thereof |
| CN109653025A (en) * | 2018-12-12 | 2019-04-19 | 济宁明升新材料有限公司 | A kind of preparation method of natural polysaccharide and its derivative modified wet strengthening agents for papermaking |
| CN113087898A (en) * | 2021-04-15 | 2021-07-09 | 浙江九本环保技术有限公司 | Preparation method and application of polyamide polyamine-polyester block type low-organochlorine wet strength agent |
-
2012
- 2012-11-09 CN CN201210445339.3A patent/CN103806337A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017207A (en) * | 2014-06-12 | 2014-09-03 | 上海东升新材料有限公司 | Paper making/breaking control agent and preparation method thereof |
| CN109208382A (en) * | 2018-11-07 | 2019-01-15 | 济宁明升新材料有限公司 | A kind of wet strengthening agents for papermaking and preparation method thereof |
| CN109653025A (en) * | 2018-12-12 | 2019-04-19 | 济宁明升新材料有限公司 | A kind of preparation method of natural polysaccharide and its derivative modified wet strengthening agents for papermaking |
| CN113087898A (en) * | 2021-04-15 | 2021-07-09 | 浙江九本环保技术有限公司 | Preparation method and application of polyamide polyamine-polyester block type low-organochlorine wet strength agent |
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Application publication date: 20140521 |