CN101509213A - Bisamide quaternary ammonium salt sheet softening agent, preparation and uses thereof - Google Patents
Bisamide quaternary ammonium salt sheet softening agent, preparation and uses thereof Download PDFInfo
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- CN101509213A CN101509213A CNA200910048399XA CN200910048399A CN101509213A CN 101509213 A CN101509213 A CN 101509213A CN A200910048399X A CNA200910048399X A CN A200910048399XA CN 200910048399 A CN200910048399 A CN 200910048399A CN 101509213 A CN101509213 A CN 101509213A
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- paper
- diethylenetriamine
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- bisamide
- quaternary ammonium
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Abstract
The invention relates to a bisamide quaternary ammonium salt paper softening agent, a preparation method and application thereof. The raw material consists of tristearin, diethylenetriamine and dimethyl sulfate. The preparation method comprises the following steps: firstly, adding the tristearin into a container, heating and dissolving the tristearin, then adding a certain amount of paratoluenesulfonic acid catalyst, stirring the mixture and raising the temperature to 130 DEG C, dripping the diethylenetriamine, continuously raising the temperature to 150 DEG C after the dripping of the diethylenetriamine is finished, and separating the diethylenetriamine to obtain an intermediate product; then putting the intermediate product into the container, and heating the intermediate product to 95 DEG C; and gradually dripping the dimethyl sulfate, preserving heat, and discharging and cooling to obtain the bisamide quaternary ammonium salt paper softening agent. The bisamide quaternary ammonium salt paper softening agent can be used for toilet paper, napkin paper, cosmetic paper, towel tissue, diaper paper and the like; and during the preparation, the synthetic process is simple, and the raw material is easily obtained. During the preparation, the paratoluenesulfonic acid catalyst can remarkably accelerate the rate of amidation reaction and shorten the reaction time, and has the function of solubilizing.
Description
Technical field
The invention belongs to the auxiliary chemicals technical field, be specifically related to a kind of bisamide quaternary ammonium salt sheet softening agent and its production and application.
Background technology
Along with people increase day by day to the demand of paper for daily use, the quality requirement to paper is also more and more higher simultaneously, especially the paper flexibility is had higher requirement.Because of containing a plurality of hydroxyls in the paper fiber molecule chain, and be the big molecule of straight chain type, interchain forms very strong molecular separating force and hydrogen bond, so paper has certain intensity and rigidity, by adding mechanisms such as various auxiliary agents and making beating, can make fiber molecule disperse, degrade and reduction degree of crystallinity, play certain soft effect that helps, but can not fundamentally solve the paper flexibility problems.Make the paper softness, the interaction force between fiber molecule is wherein reduced, segment and strand can both be moved.
And the paper softener great majority are to contain C
16The surfactant of above hydrophobic group under appropriate processing condition, on the surface attached to fiber, can form the hydrophobic membrane of parcel fiber, thereby the paper flexibility is improved; And reduce the frictional force of paper to skin, increase smooth, the fine and smooth sensation of paper; Thereby obtain the feel of smooth, soft.
At present, softening agent for paper mainly contains organosilicon macromolecule, wax latex, metal complex etc.Though organosilicon macromolecule softener soft effect is good, cost of material is higher.The emulsifying wax softener is mainly used in paraffin paper and waterproof paper, and the water imbibition of paper is relatively poor.Metal complex mainly is metals such as chromium, zirconium, can not use on paper for daily use.
Summary of the invention
The present invention has proposed a kind of new bisamide quaternary ammonium salt sheet softening agent in order to solve as above problem.
Bisamide quaternary ammonium salt sheet softening agent belongs to a kind of cationic surfactant of special construction, has soft effect preferably.Because cationic softener is positively charged, and fiber is had high affinity, on fiber surface, evenly adsorb and formation one deck oil film, thereby make fiber surface smooth, greasy feeling is arranged.And fiber fines and the filler in the fine slurry of paper had the retention effect, fiber fines, filler can be filled between the long fiber, make long fiber be evenly distributed, interweaving property and regularity improve, the paper that is ferreted out has good flexibility and bulkiness, the dry linting of paper, fall a mao phenomenon and reduced, also have the fungus and mildew resistance effect simultaneously.
Know-why of the present invention
The first step, amidation process
Second step, quaterisation
A kind of bisamide quaternary ammonium salt sheet softening agent, raw material consists of:
Tristerin, diethylenetriamine and dimethyl suflfate, the mol ratio that its raw material is formed is pressed: tristerin: diethylenetriamine: dimethyl suflfate=2:3:3.
A kind of preparation of bisamide quaternary ammonium salt sheet softening agent comprises being prepared as follows step:
(1), raw material is prepared: get tristerin, diethylenetriamine and dimethyl suflfate, the mol ratio that its raw material is formed is pressed: tristerin: diethylenetriamine: dimethyl suflfate=2:3:3;
(2), amidation process: the ready raw material tristerin of step (1) is added in the container, after being heated to 60 ℃ of dissolvings, the Catalyzed by p-Toluenesulfonic Acid agent that adds the mass fraction 1.2% that accounts for raw material, stir, rotating speed is 120r/min, is warmed up to 130 ℃ again, drip the ready raw material diethylenetriamine of step (1), after dripping diethylenetriamine, continue to be warmed up to 150 ℃, insulation reaction 2～2.5h; By the moisture content separator, separate moisture content, obtain intermediate;
(3), quaterisation: the intermediate that obtains in the step (2) is put into container, be warmed up to 90 ℃; Drip the ready raw material sulphuric acid dimethyl ester of step (1) gradually, insulation reaction 1～1.5h, the discharging cooling obtains light yellow block product, is bisamide quaternary ammonium salt sheet softening agent of the present invention.
Beneficial effect of the present invention
Bisamide quaternary ammonium salt sheet softening agent of the present invention can be used for toilet paper, napkin paper, beauty treatment paper, napkin, urine towel paper etc., and in the bisamide quaternary ammonium salt sheet softening agent preparation process, synthesis technique is simple, and raw material is easy to get.Use the Catalyzed by p-Toluenesulfonic Acid agent in the preparation process, can obviously accelerate rate of amidation reaction, shorten the reaction time, and have solubilization.
The specific embodiment
Set forth the present invention with specific embodiment below, but do not limit the present invention.
Embodiment 1
The tristerin adding of 130g is equipped with in the there-necked flask of agitator, thermometer, after being heated to 60 ℃ of dissolvings, the Catalyzed by p-Toluenesulfonic Acid agent that adds the mass fraction 1.2% that accounts for raw material, stir, rotating speed is 120r/min, be warmed up to 130 ℃ after, drip the diethylenetriamine of 33g, after dripping diethylenetriamine, be warmed up to 150 ℃ gradually, insulation reaction 2.5h; By the moisture content separator, separate moisture content, obtain intermediate.
The intermediate 146g that obtains is put into there-necked flask, be warmed up to 95 ℃; Drip the 32g dimethyl suflfate gradually, insulation reaction 1h, the discharging cooling obtains light yellow block product, is bisamide quaternary ammonium salt sheet softening agent.
The softener outward appearance is a light beige paste solid, and special odor is arranged, and cationic degree is 0.4.
Embodiment 2
The tristerin adding of 150g is equipped with in the there-necked flask of agitator, thermometer, after being heated to 60 ℃ of dissolvings, the Catalyzed by p-Toluenesulfonic Acid agent that adds the mass fraction 1.4% that accounts for raw material, after stirring is warmed up to 130 ℃, drip the diethylenetriamine of 44g, after dripping diethylenetriamine, be warmed up to 150 ℃ gradually, insulation reaction 2h; By the moisture content separator, separate moisture content, obtain intermediate.
Above-mentioned intermediate 173g is put into there-necked flask, be warmed up to 95 ℃; Drip the 39g dimethyl suflfate gradually, the insulation reaction 1.5h time, the discharging cooling obtains light yellow block product, is bisamide quaternary ammonium salt sheet softening agent.
The softener outward appearance is a light beige paste solid, and special odor is arranged, and cationic degree is 0.6.
Embodiment 3
The application of bisamide quaternary ammonium salt sheet softening agent
Copy paper and test 100% bleached wheat straw pulp that used paper pulp provides for certain paper plant, 30 ° of SR of beating degree.Before experiment,, remove foreign material such as screenings through simple screening.
Load weighted softener added in a certain amount of hot water dissolve, with small-sized beater or homogenizer disperse, emulsification, make the slurry of solid content 15%, again with it by 6 softener slurries: 1000 straw pulps (mass ratio) add in the machine chest and stir, copy paper after leaving standstill certain hour, measure respectively paper quantitatively, whiteness, tensile strength and pliability, test result sees the following form 1.
The performance test of table 1, softener
As shown in Table 1, add the bisamide quaternary ammonium salt softener in paper, can make paper become soft, soft effect is best when the consumption of softener is 0.4%～0.8%.Fiber surface tension force is descended, and fiber surface becomes and is easy to expansion, significantly improves the softness and the bulkiness of paper, produces soft feel.When the consumption of softener surpasses after 0.8%, when increasing the consumption of softener again, little to the influence of paper soft effect.But increase along with the softener consumption, in softness that significantly improves paper and bulkiness, paper of whiteness there is no obvious variation, but the paper tensile strength obviously reduces, and this is because the electrical absorption of softener and fiber has destroyed the hydrogen bond association between the fiber.Find out that thus paper flexibility and its tensile strength are conflicting, but the softener consumption is in 0.4%～0.8% scope the time, it is not very big that tensile strength descends.
Selecting the softener cationic degree for use is 0.4, and consumption is 0.6%, does under same experimental conditions with Russian softener and copies the paper contrast test, measures the paper pliability.And being converted into soft effect, experimental result sees the following form 2.
The application of table 2, softener
Annotate: soft effect=the do not add paper pliability of the paper pliability/interpolation softener of softener
As known from Table 2, behind the interpolation bisamide quaternary ammonium salt sheet softening agent, the softness values of paper reduces in paper, and softness improves, and the page feel is satiny, dry and comfortable, has overcome dry linting and has fallen a mao phenomenon, and guaranteed paper of whiteness.Drawing bisamide quaternary ammonium salt thus is comparatively ideal paper softener.And this softener synthesis technique is simple, and raw material is easy to get.
Claims (3)
1, a kind of bisamide quaternary ammonium salt sheet softening agent is characterized in that raw material consists of: tristerin, diethylenetriamine and dimethyl suflfate, the mol ratio that its raw material is formed: tristerin: diethylenetriamine: dimethyl suflfate=2:3:3.
2, a kind of preparation method of a kind of bisamide quaternary ammonium salt sheet softening agent as claimed in claim 1 is characterized in that comprising being prepared as follows step:
(1), raw material is prepared: get tristerin, diethylenetriamine and dimethyl suflfate, the mol ratio that its raw material is formed is pressed: tristerin: diethylenetriamine: dimethyl suflfate=2:3:3;
(2), amidation process: the ready raw material tristerin of step (1) is added in the container, after being heated to 60 ℃ of dissolvings, the Catalyzed by p-Toluenesulfonic Acid agent that adds the mass fraction 1.2% that accounts for raw material, stir, rotating speed is 120r/min, is warmed up to 130 ℃ again, drip the ready raw material diethylenetriamine of step (1), after dripping diethylenetriamine, continue to be warmed up to 150 ℃, insulation reaction 2～2.5h; By the moisture content separator, separate moisture content, obtain intermediate;
(3), quaterisation: the intermediate that obtains in the step (2) is put into container, be warmed up to 90 ℃; Drip the ready raw material sulphuric acid dimethyl ester of step (1) gradually, insulation reaction 1～1.5h, the discharging cooling obtains light yellow block product, is bisamide quaternary ammonium salt sheet softening agent of the present invention.
3, a kind of bisamide quaternary ammonium salt sheet softening agent as claimed in claim 1 is characterized in that can be used for the paper of copying of toilet paper, napkin paper, beauty treatment paper, napkin, urine towel paper, and consumption is 0.4%～0.8%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200910048399XA CN101509213A (en) | 2009-03-27 | 2009-03-27 | Bisamide quaternary ammonium salt sheet softening agent, preparation and uses thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CNA200910048399XA CN101509213A (en) | 2009-03-27 | 2009-03-27 | Bisamide quaternary ammonium salt sheet softening agent, preparation and uses thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104120626A (en) * | 2014-07-10 | 2014-10-29 | 九洲生物技术（苏州）有限公司 | A sizing agent, a preparing method thereof and applications of the sizing agent |
| CN104389232A (en) * | 2014-10-23 | 2015-03-04 | 广东比伦生活用纸有限公司 | Super-soft perfuming household paper and production method thereof |
| CN104404818A (en) * | 2014-10-23 | 2015-03-11 | 广东比伦生活用纸有限公司 | Super soft coil paper and production method thereof |
| CN104452429A (en) * | 2014-10-23 | 2015-03-25 | 广东比伦生活用纸有限公司 | Super-soft super-tough household paper and production method thereof |
-
2009
- 2009-03-27 CN CNA200910048399XA patent/CN101509213A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104120626A (en) * | 2014-07-10 | 2014-10-29 | 九洲生物技术（苏州）有限公司 | A sizing agent, a preparing method thereof and applications of the sizing agent |
| CN104389232A (en) * | 2014-10-23 | 2015-03-04 | 广东比伦生活用纸有限公司 | Super-soft perfuming household paper and production method thereof |
| CN104404818A (en) * | 2014-10-23 | 2015-03-11 | 广东比伦生活用纸有限公司 | Super soft coil paper and production method thereof |
| CN104452429A (en) * | 2014-10-23 | 2015-03-25 | 广东比伦生活用纸有限公司 | Super-soft super-tough household paper and production method thereof |
| CN104404818B (en) * | 2014-10-23 | 2016-08-24 | 广东比伦生活用纸有限公司 | A kind of ultra-toughness coil paper and production method thereof |
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Open date: 20090819 |