CN104327264B - Preparation method with odor type surfactant - Google Patents
Preparation method with odor type surfactant Download PDFInfo
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- CN104327264B CN104327264B CN201410535706.8A CN201410535706A CN104327264B CN 104327264 B CN104327264 B CN 104327264B CN 201410535706 A CN201410535706 A CN 201410535706A CN 104327264 B CN104327264 B CN 104327264B
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Abstract
The present invention relates to the preparation method of a kind of band odor type surfactant, belong to surfactant preparing technical field.The preparation method of band odor type surfactant of the present invention, is made up of the raw material of following parts by weight: initiator 50 100 parts, catalyst 13 parts, expoxy propane 200 800 parts, and described initiator is anisyl alcohol.Preparation method of the present invention is scientific and reasonable, simple, and the product of preparation is with natural scents, asepsis environment-protecting.
Description
Technical field
The present invention relates to the preparation method of a kind of band odor type surfactant, belong to surfactant preparing technical field.
Background technology
Along with growth in the living standard, people have the highest requirement for quality of life.Dress ornament, food, daily use chemicals etc. are pacified
Full problems demand solves.Nonylphenol class surfactant conventional in tradition daily use chemicals, alkyl benzene sulphonate sodium salt, alkyl phenol polyoxy second
Although alkene ether etc. has a good dirt-removing power, but have that biodegradability is poor, Long contact time affects the shortcomings such as health.
Tradition detergent compound essence, strong flavor, Long contact time can cause allergic reaction, and causes various diseases.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of band odor type surfactant, it is scientific and reasonable, simple, preparation
Product with natural scents, asepsis environment-protecting.
The preparation method of band odor type surfactant of the present invention, it is characterised in that be made up of the raw material of following parts by weight:
Initiator 50-100 part, catalyst 1-3 part, expoxy propane 200-800 part, described initiator is anisyl alcohol.
Described catalyst is base metal catalysts, bimetallic cyanide complex catalyst or phosphonitrile class catalyst.
The preferred potassium hydroxide of base metal catalysts；Bimetallic cyanide complex catalyst preferred bimetallic polyethers catalyst MMC；
The preferred hexachlorocyclotriph,sphazene of phosphonitrile class catalyst.
The preparation method of described band odor type surfactant, including following preparation process: by anisyl alcohol with catalyst dissolution to all
Phase, solution temperature is 50-70 DEG C, displacement, heats up, and instills propylene oxide reaction and prepares thick polyethers；Thick polyethers through washing, neutralize,
Absorption, dry, the prepared finished product polyethers of filtration.
Described reaction is warming up to 80-110 DEG C, and the response time is 8-16h.
Anise alcohol, formal name used at school para-methoxybenzyl alcohol, nontoxic, polyether polyol prepared therefrom, there is similar Flos Caryophylli, vanilla temperature
The fragrance of a flower fragrance of sum, can make surfactant in the industry such as cosmetics, daily use chemicals and use.And due to anise alcohol self with
Fragrance, it is possible to reduce or save the use of compound essence, thus reduce the probability that human body is ill.
The method have the advantages that
(1) raw materials used low cost, asepsis environment-protecting；
(2) due to anise alcohol self with fragrance, the use of compound essence can be reduced or eliminated, reduce the probability that human body is ill；
(3) preparation method is scientific and reasonable, simple possible.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated, but it is not limiting as the enforcement of the present invention.
Raw materials used it is commercially available prod.
Embodiment 1
(1) accurately weigh 50g anisyl alcohol and 1.1g potassium hydroxide catalyst, move in polymeric kettle.
(2) starting stirring, nitrogen is replaced 3 times, is to slowly warm up to 50 DEG C and is dissolved to homogeneous.
(3) it is continuously heating to 87 DEG C, after being slowly dropped into 12g expoxy propane, stops charging.
(4), after question response starts polymerization, use continuous feed mode to add residue 188g expoxy propane and prepare thick polyethers.Reaction
Temperature is 100 ± 5 DEG C, reacts 8h, and reaction pressure is 0.2MPa.
(5) thick polyethers is cooled to 79 DEG C, adds water and phosphoric acid, be adjusted to pH=6.0.
(6) adding activated carbon to adsorb, be warming up to 110 DEG C of logical nitrogen evacuation and anhydrate, circulating filtration prepares finished product polyethers.
Finished product index: hydroxyl value 60.2mgKOH/g, acid number 0.042mgKOH/g, moisture 0.038%, potassium ion 3ppm, color
Value 50 (APHA), pH 6.01.
Embodiment 2
(1) accurately weigh 100g anisyl alcohol and 2.2g bimetallic polyethers catalyst MMC, move in polymeric kettle.
(2) starting stirring, nitrogen is replaced 4 times, is to slowly warm up to 70 DEG C and is dissolved to homogeneous.
(3) it is continuously heating to 84 DEG C, after being slowly dropped into 56g expoxy propane, stops charging.
(4), after question response starts polymerization, use continuous feed mode to add residue 744g expoxy propane and prepare thick polyethers.Reaction
Temperature is 85 ± 5 DEG C, reacts 16h, and reaction pressure is 0.2MPa.
(5) thick polyethers is cooled to 82 DEG C, adds water and phosphoric acid, be adjusted to pH=6.8.
(6) adding activated carbon to adsorb, be warming up to 100 DEG C of logical nitrogen evacuation and anhydrate, circulating filtration prepares finished product polyethers.
Finished product index: hydroxyl value 66.4mgKOH/g, acid number 0.061mgKOH/g, moisture 0.048%, potassium ion 5ppm, color
Value 70 (APHA), pH 6.87.
Embodiment 3
(1) accurately weigh 80g anisyl alcohol and 1.74g hexachlorocyclotriph,sphazene catalyst, move in polymeric kettle.
(2) starting stirring, nitrogen is replaced 3 times, is to slowly warm up to 61 DEG C and is dissolved to homogeneous.
(3) it is continuously heating to 90 DEG C, after being slowly dropped into 30g expoxy propane, stops charging.
(4), after question response starts polymerization, use continuous feed mode to add residue 470g expoxy propane and prepare thick polyethers.Reaction
Temperature is 90 ± 5 DEG C, reacts 10h, and reaction pressure is 0.1MPa.
(5) thick polyethers is lowered the temperature 87 DEG C, add water and phosphoric acid, be adjusted to pH=5.5.
(6) adding activated carbon to adsorb, be warming up to 105 DEG C of logical nitrogen evacuation and anhydrate, circulating filtration prepares finished product polyethers.
Finished product index: hydroxyl value 59.8mgKOH/g, acid number 0.033mgKOH/g, moisture 0.019%, potassium ion 2ppm, color
Value 30 (APHA), pH 5.51.
Claims (5)
1. the preparation method of a band odor type surfactant, it is characterised in that be made up of the raw material of following parts by weight: initiator
50-100 part, catalyst 1-3 part, expoxy propane 200-800 part, described initiator is anisyl alcohol；Catalyst is bimetallic
Cyanide complex catalyst or phosphonitrile class catalyst.
The preparation method of band odor type surfactant the most according to claim 1, it is characterised in that: double metal cyanide network
Mixture catalyst is bimetallic polyethers catalyst MMC；Phosphonitrile class catalyst is hexachlorocyclotriph,sphazene.
The preparation method of band odor type surfactant the most according to claim 1 and 2, it is characterised in that include following preparation
Step: by anisyl alcohol with catalyst dissolution to homogeneously, heat up, instill propylene oxide reaction and prepare thick polyethers；Thick polyethers is through water
Wash, neutralize, adsorb, be dried, filter prepared finished product polyethers.
The preparation method of band odor type surfactant the most according to claim 3, it is characterised in that: solution temperature is
50-70℃。
The preparation method of band odor type surfactant the most according to claim 3, it is characterised in that: it is warming up to 80-110 DEG C,
Response time is 8-16h.
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| CN201410535706.8A CN104327264B (en) | 2014-10-11 | 2014-10-11 | Preparation method with odor type surfactant |
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| CN201410535706.8A CN104327264B (en) | 2014-10-11 | 2014-10-11 | Preparation method with odor type surfactant |
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| CN104327264B true CN104327264B (en) | 2016-08-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104910370A (en) * | 2015-06-11 | 2015-09-16 | 山东一诺威新材料有限公司 | Preparation method of high-activity low-unsaturation-degree polyether polyol for shoe materials |
| CN105237759B (en) * | 2015-11-09 | 2017-07-07 | 淄博德信联邦化学工业有限公司 | Tensile elasticity body PPG high and preparation method thereof |
| CN106188521B (en) * | 2016-07-30 | 2018-07-10 | 淄博德信联邦化学工业有限公司 | Synthesis of polymer polyalcohol macromolecule dispersing agent |
| CN108823003A (en) * | 2018-06-19 | 2018-11-16 | 浙江永金生物科技有限公司 | Low bubble dish washing liquid of a kind of hyperconcetration green and preparation method thereof |
Citations (2)
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| CN1233282A (en) * | 1996-08-19 | 1999-10-27 | 普罗格特-甘布尔公司 | Laundry detergent compositions comprising 'beta'-ketoester pro-fragrances |
| CN1701057A (en) * | 2002-09-18 | 2005-11-23 | 巴斯福股份公司 | Method for producing alkoxylated products at optimized reaction pressures |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1061027A (en) * | 1990-10-20 | 1992-05-13 | 中国石油化工总公司兰州炼油化工总厂 | The preparation of milky active initiator during polyethers is produced |
| US5426174A (en) * | 1992-12-08 | 1995-06-20 | Arco Chemical Technology, L.P. | Hydroxy-functionalized polyoxyalkylene ether compositions derived from mixtures of C4 epoxides |
| JP4036566B2 (en) * | 1999-05-18 | 2008-01-23 | 三井化学株式会社 | Process for producing polyalkylene oxide |
| EP2015014A1 (en) * | 2007-07-11 | 2009-01-14 | Bayer MaterialScience AG | Method for drying foams made of aqueous PUR dispersions |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1233282A (en) * | 1996-08-19 | 1999-10-27 | 普罗格特-甘布尔公司 | Laundry detergent compositions comprising 'beta'-ketoester pro-fragrances |
| CN1701057A (en) * | 2002-09-18 | 2005-11-23 | 巴斯福股份公司 | Method for producing alkoxylated products at optimized reaction pressures |
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Denomination of invention: Preparation method of fragrant surfactant Effective date of registration: 20211201 Granted publication date: 20160817 Pledgee: Qi Shang bank Limited by Share Ltd. Huantai branch Pledgor: ZIBO DEXIN LIANBANG CHEMICAL INDUSTRY Co.,Ltd. Registration number: Y2021980013724 |