CN101225060A - Method for synthesizing aliphatic amine polyoxyethylene ether ammonium sulfate - Google Patents
Method for synthesizing aliphatic amine polyoxyethylene ether ammonium sulfate Download PDFInfo
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- CN101225060A CN101225060A CNA2007101647964A CN200710164796A CN101225060A CN 101225060 A CN101225060 A CN 101225060A CN A2007101647964 A CNA2007101647964 A CN A2007101647964A CN 200710164796 A CN200710164796 A CN 200710164796A CN 101225060 A CN101225060 A CN 101225060A
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- polyoxyethylene ether
- aliphatic amine
- amine polyoxyethylene
- ammonium sulfate
- ether ammonium
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Abstract
The invention discloses a synthesis method for aliphatic amine polyoxyethylene ether ammonium sulfate, belonging to technical field of synthesizing sulfate ester type amphoteric surface-active material in organic chemistry, which is characterized in that: aliphatic amine polyoxyethylene ether is used as raw material; sulfamic acid is used as sulfation reagent; urea is used as catalyst; aliphatic amine polyoxyethylene ether is neutralized under the protection of nitrogen before sulfated with sulfamic acid under the catalysis of the urea; deionized water is finally added and stirred to get aliphatic amine polyoxyethylene ether ammonium sulfate; the molar ration between the aliphatic amine polyoxyethylene ether and the sulfamic acid is 1 : 1.0 to 1.8; the molar ration between the aliphatic amine polyoxyethylene ether and the urea is 1 : 0.2 to 1.0. The synthesis method reasonably selects the sulfamic acid as sulfation reagent and the urea as catalyst to make sulfation modification upon aliphatic amine polyoxyethylene ether and synthesize aliphatic amine polyoxyethylene ether ammonium sulfate. The synthesis method for aliphatic amine polyoxyethylene ether ammonium sulfate has the advantages of simple technique, small side reaction and mild reaction condition.
Description
Technical field
The present invention relates to a kind of synthetic method of aliphatic amine polyoxyethylene ether ammonium sulfate, belong to the synthesis technical field of sulfuric acid ester type amphoterics in the organic chemistry.
Background technology
In each operation of textile dyeing and finishing, detergent all has extensive use.Come unstuck in the refining that the destarch of fabric and kiering, synthon are removed degreasing, fine, soft fur and washing in finish, the woolen industry, raw silk, eccysis all will not used detergent in the back arrangement of the dye well fabric of fixation behind textile dyeing and the stamp.
At present, used detergent mainly is anion surfactant and nonionogenic tenside in textile industry.Anion surfactant cooperates detersive power good with alkali, and it is relatively good to wash the back fabric feeling.The nonionogenic tenside detersive power is big, even detersive power is also very strong under lower concentration; And foam is few, easily makes liquid washing agent; In water, do not dissociate, all relatively insensitive to hard water and ionogen; Micelle-forming concentration is very low, has good characteristic of solubilizing; Biological degradability is good.Above-mentioned detergent kind is more, and does not mostly have particular requirement when using.But these detergents have also that a fatal shortcoming---specificity is poor.
Summary of the invention
It is reasonable that the object of the invention provides a kind of technology, has the synthetic method of the aliphatic amine polyoxyethylene ether ammonium sulfate of better application performance.
The present invention is the synthetic method of aliphatic amine polyoxyethylene ether ammonium sulfate; with the aliphatic amine polyoxyethylene ether is raw material; it is characterized in that with the thionamic acid being sulfur acidizing reagent, urea is catalyzer, under nitrogen protection; aliphatic amine polyoxyethylene ether is after the acid neutralization is for neutrality; under the urea seeding effect,, add deionized water at last with thionamic acid generation sulfating reaction; stir, obtain aliphatic amine polyoxyethylene ether ammonium sulfate.
The carbonatoms of described aliphatic amine polyoxyethylene ether carbochain can be 12～18.
The polyoxyethylene adduct number of described aliphatic amine polyoxyethylene ether can be controlled in 2～30.
Describedly be used for neutral acid and can be sulfuric acid or hydrochloric acid, acetate etc.
The mol ratio of described aliphatic amine polyoxyethylene ether and thionamic acid can be 1: 1.0～and 1.8.
The mol ratio of described aliphatic amine polyoxyethylene ether and urea can be 1: 0.2～and 1.0.
The temperature of reaction of described sulfating reaction can be 110～160 ℃.
The reaction times of described sulfating reaction can be 2～6 hours.
The content of described aliphatic amine polyoxyethylene ether ammonium sulfate finished product can be 20%～70%, and this can be as required, and the add-on of control deionized water is regulated.
The present invention compared with prior art has following outstanding advantage and positively effect:
1, rationally selecting thionamic acid for use is sulfur acidizing reagent, and urea is catalyzer, and aliphatic amine polyoxyethylene ether is carried out the sulfation modification, the synthetic fatty amine polyoxyethylene ether ammonium sulfate, and technology is simple, side reaction is few.
2, through optimization design and repetition test research, rationally determined processing parameter and conditions such as proportioning raw materials, catalyst levels, sulfating reaction temperature, time, the reaction conditions gentleness, institute's employing equipment is simple, is fit to batch production, and facility investment is few.
3, by synthetic aliphatic amine polyoxyethylene ether ammonium sulfate of the present invention, the advantage that integrates anion surfactant and nonionogenic tenside two class detergents, have lighter color, the excellent characteristics of quality, have performances such as favorable biological degradability, detersive power, whipability and emulsification, dispersion, infiltration, be applicable to fields such as textile printing and dyeing, daily use chemicals washing.Can be used as the new type amphoteric surfactant detergent, be used for the good washing composition of article such as wool, eider down, under room temperature or low temperature, use, owing in the aqueous solution, also show weak cation, give fabric fluffy, soft hand feeling after the washing, non-stimulated to skin, also can improve the wool fulling milling.Be used for eider down cleaning by degreasing technology, only need a procedure can reach the degreasing soft effect, wool, eider down are sterilized simultaneously, insect-free in the future.Also can be used as metal cleaner.
Embodiment
Embodiment 1: add 10mol primary octadecylamine polyoxyethylene (15) ether in reactor, add sulfuric acid and be neutralized to neutrality.Add 16mol thionamic acid, 0.6mol urea then, feed nitrogen, be heated to 115～125 ℃, insulation reaction 1.5h.Be warmed up to 135～140 ℃ then, insulation reaction 2.0h.Insulation cools to 80～90 ℃ after finishing, and adds the dilution of 936mol deionized water, stirs 2.0h in 75～85 ℃.Be cooled to 60～70 ℃ of blowings, obtain content and be 40% red-brown transparent liquid, be primary octadecylamine polyoxyethylene (15) ether ammonium sulfate.
The chemical equation of sulfating reaction is in the above-mentioned enforcement:
Embodiment 2: add 10mol ten di-primary amine polyoxyethylene (2) ethers in reactor, add hydrochloric acid and be neutralized to neutrality, vacuum is sloughed moisture then.Add 13mol thionamic acid, 3mol urea, feed nitrogen, be heated to 115～125 ℃, insulation reaction 1.5h.Be warmed up to 135～140 ℃ then, insulation reaction 2.0h.Insulation cools to 80～90 ℃ after finishing, and adds the dilution of 170mol deionized water, stirs 2.0h in 75～85 ℃.Be cooled to 60～70 ℃ of blowings, obtain content and be 60% ten di-primary amine polyoxyethylene (2) ether ammonium sulfates.
The present invention is not limited to the foregoing description, when practical application, can require and use occasion according to the different performance of aliphatic amine polyoxyethylene ether ammonium sulfate, select the different proportionings in the foregoing description, or the different proportionings except that the various embodiments described above, but all do not limit the scope of the invention in any form.
Claims (9)
1. the synthetic method of an aliphatic amine polyoxyethylene ether ammonium sulfate; with the aliphatic amine polyoxyethylene ether is raw material; it is characterized in that with the thionamic acid being sulfur acidizing reagent, urea is catalyzer, under nitrogen protection; aliphatic amine polyoxyethylene ether is after the acid neutralization is for neutrality; under the urea seeding effect,, add deionized water at last with thionamic acid generation sulfating reaction; stir, obtain aliphatic amine polyoxyethylene ether ammonium sulfate.
2. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, the carbonatoms that it is characterized in that described aliphatic amine polyoxyethylene ether carbochain is 12～18.
3. by the synthetic method of claim 1 or 2 described aliphatic amine polyoxyethylene ether ammonium sulfates, it is characterized in that the polyoxyethylene adduct number of described aliphatic amine polyoxyethylene ether is controlled at 2～30.
4. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, it is characterized in that describedly being used for neutral acid and being sulfuric acid or hydrochloric acid, acetate.
5. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, the mol ratio that it is characterized in that described aliphatic amine polyoxyethylene ether and thionamic acid is 1: 1.0～1.8.
6. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, the mol ratio that it is characterized in that described aliphatic amine polyoxyethylene ether and urea is 1: 0.2～1.0.
7. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, the temperature of reaction that it is characterized in that described sulfating reaction is 110～160 ℃.
8. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, the reaction times that it is characterized in that described sulfating reaction is 2～6 hours.
9. by the synthetic method of the described aliphatic amine polyoxyethylene ether ammonium sulfate of claim 1, the content that it is characterized in that described aliphatic amine polyoxyethylene ether ammonium sulfate finished product is 20%～70%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101647964A CN101225060A (en) | 2007-12-21 | 2007-12-21 | Method for synthesizing aliphatic amine polyoxyethylene ether ammonium sulfate |
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| CNA2007101647964A CN101225060A (en) | 2007-12-21 | 2007-12-21 | Method for synthesizing aliphatic amine polyoxyethylene ether ammonium sulfate |
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| CN101225060A true CN101225060A (en) | 2008-07-23 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107164114A (en) * | 2017-05-23 | 2017-09-15 | 浙江丝科院轻纺材料有限公司 | A kind of antifouling soaping agent of the quaternary ammonium salt of chain containing APEO and preparation method thereof |
| CN109267393A (en) * | 2018-07-26 | 2019-01-25 | 浙江丝科院轻纺材料有限公司 | A kind of preparation method of the oil removing level dyeing compound emulsifying agent for dacron |
| CN109577008A (en) * | 2018-11-12 | 2019-04-05 | 山东华晨彩装科技有限公司 | A kind of high-efficiency refining agent and its preparation method and application for pure cotton fabric continuously or intermittently boiling |
| CN111657278A (en) * | 2020-05-06 | 2020-09-15 | 南京威尔生物科技有限公司 | Glufosinate-ammonium assistant, glufosinate-ammonium aqueous solution prepared by using glufosinate-ammonium assistant and preparation method of glufosinate-ammonium aqueous solution |
| CN111732525A (en) * | 2020-07-31 | 2020-10-02 | 湖南丽臣奥威实业有限公司 | Method for preparing non-aqueous system fatty alcohol ether sulfuric acid organic alkanolamine salt product |
| CN114213647A (en) * | 2021-11-30 | 2022-03-22 | 厦门大邦瑞达印染材料有限公司 | Zwitterionic surfactant, preparation method and application thereof |
| CN114957048A (en) * | 2022-06-30 | 2022-08-30 | 浙江皇马科技股份有限公司 | General preparation method of polystyrylphenol polyoxyethylene ether ammonium sulfate |
-
2007
- 2007-12-21 CN CNA2007101647964A patent/CN101225060A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107164114A (en) * | 2017-05-23 | 2017-09-15 | 浙江丝科院轻纺材料有限公司 | A kind of antifouling soaping agent of the quaternary ammonium salt of chain containing APEO and preparation method thereof |
| CN109267393A (en) * | 2018-07-26 | 2019-01-25 | 浙江丝科院轻纺材料有限公司 | A kind of preparation method of the oil removing level dyeing compound emulsifying agent for dacron |
| CN109577008A (en) * | 2018-11-12 | 2019-04-05 | 山东华晨彩装科技有限公司 | A kind of high-efficiency refining agent and its preparation method and application for pure cotton fabric continuously or intermittently boiling |
| CN111657278A (en) * | 2020-05-06 | 2020-09-15 | 南京威尔生物科技有限公司 | Glufosinate-ammonium assistant, glufosinate-ammonium aqueous solution prepared by using glufosinate-ammonium assistant and preparation method of glufosinate-ammonium aqueous solution |
| CN111732525A (en) * | 2020-07-31 | 2020-10-02 | 湖南丽臣奥威实业有限公司 | Method for preparing non-aqueous system fatty alcohol ether sulfuric acid organic alkanolamine salt product |
| CN114213647A (en) * | 2021-11-30 | 2022-03-22 | 厦门大邦瑞达印染材料有限公司 | Zwitterionic surfactant, preparation method and application thereof |
| CN114957048A (en) * | 2022-06-30 | 2022-08-30 | 浙江皇马科技股份有限公司 | General preparation method of polystyrylphenol polyoxyethylene ether ammonium sulfate |
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Open date: 20080723 |