CN106748897B - A kind of serialization prepares the method and apparatus of fatty alkyl amidopropyl amine oxide - Google Patents
A kind of serialization prepares the method and apparatus of fatty alkyl amidopropyl amine oxide Download PDFInfo
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- CN106748897B CN106748897B CN201611244120.1A CN201611244120A CN106748897B CN 106748897 B CN106748897 B CN 106748897B CN 201611244120 A CN201611244120 A CN 201611244120A CN 106748897 B CN106748897 B CN 106748897B
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- fixed bed
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- amine oxide
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- 150000001412 amines Chemical class 0.000 title claims abstract description 20
- 125000000217 alkyl group Chemical group 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000007789 gas Substances 0.000 claims abstract description 31
- 239000007800 oxidant agent Substances 0.000 claims abstract description 23
- 230000001590 oxidative effect Effects 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 230000003068 static effect Effects 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- 230000009471 action Effects 0.000 claims abstract description 3
- 238000004064 recycling Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 8
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 7
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 239000003622 immobilized catalyst Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004480 active ingredient Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- -1 propyl tertiary amine Chemical class 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 239000012071 phase Substances 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 239000011344 liquid material Substances 0.000 abstract description 3
- 125000003277 amino group Chemical group 0.000 abstract 1
- 239000000047 product Substances 0.000 description 10
- 230000008676 import Effects 0.000 description 4
- 239000012263 liquid product Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002453 shampoo Substances 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002979 fabric softener Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C291/00—Compounds containing carbon and nitrogen and having functional groups not covered by groups C07C201/00 - C07C281/00
- C07C291/02—Compounds containing carbon and nitrogen and having functional groups not covered by groups C07C201/00 - C07C281/00 containing nitrogen-oxide bonds
- C07C291/04—Compounds containing carbon and nitrogen and having functional groups not covered by groups C07C201/00 - C07C281/00 containing nitrogen-oxide bonds containing amino-oxide bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The present invention relates to the method and apparatus that a kind of serialization prepares fatty alkyl amidopropyl amine oxide.The method that purpose is to provide has the characteristics that process route is succinct, and device has the characteristics that configuration is simple.Technical solution is：A kind of method that serialization prepares fatty alkyl amidopropyl amine oxide, carries out according to following steps：1) PKO, hydrogen peroxide and water are passed through in fixed bed reactors；2) gaseous oxidant enters in fixed bed reactors and is reacted under the action of catalyst in fixed bed reactors with gaseous oxidant with PKO, hydrogen peroxide；3) material is after the output of gas-liquid separation fixed bed reactors after the completion of reacting, through gas-liquid separator separates material；Wherein gas phase returns to the recycling of gas buffer tank as gaseous oxidant, and liquid phase is amine oxide product.A kind of continuous device for preparing fatty alkyl amidopropyl amine oxide, which includes liquid material entrance, static mixer, fixed bed reactors, gas-liquid separator, gas buffer tank and wind turbine.
Description
Technical field
The present invention relates to field of fine chemical, and in particular to a kind of serialization prepares fatty alkyl amidopropyl amine oxide
Method and apparatus.
Background technology
Fatty alkyl amidopropyl amine oxide (CAO) has the effects that excellent bubble, cleaning, emulsification, solubilising, thickening, to oxidation
Agent, the chemical stability of soda acid are preferable, mild to skin and eyes, have synergistic effect, environmental protection, safety with anion active agent
Also preferably, it is widely used in detergent, shampoo and fabric softener and shampoo.
The production technology of existing routine CAO, usually utilize in a kettle fatty acid amide propyl tertiary amine (PKO) with it is double
Oxygen water reacts, and in order to improve conversion ratio when production, need to increase the rate of charge of hydrogen peroxide, and must divide for the anti-material kettle hydrogen peroxide that overflows
It criticizes and feeds intake, increase the reaction time, and because of the excess of hydrogen peroxide, when leading to increase the hydrogen peroxide residue degradation in finished product
Between.
Invention content
It is an object of the present invention to provide the method and apparatus that a kind of serialization prepares fatty alkyl amidopropyl amine oxide, provide
Method have the characteristics that process route succinct, good product quality, production efficiency are high, the device provided has that configuration is simple, throws
Provide feature at low cost.
Technical solution provided by the invention is：
A kind of method that serialization prepares fatty alkyl amidopropyl amine oxide, carries out according to following steps：
1) PKO, hydrogen peroxide and water are passed through from bottom in fixed bed reactors after mixing by static mixer；It is described
Immobilized catalyst is previously added in fixed bed reactors；
2) gaseous oxidant is entered from gas buffer tank in fixed bed reactors by gas transfer pump, with PKO, hydrogen peroxide
It is reacted under the action of catalyst in fixed bed reactors with gaseous oxidant, 40~80 DEG C of controlling reaction temperature；Gas is slow
It rushes gas pressure in tank and maintains 0.1~0.5Mpa, by gaseous oxidant entrance make-up gas oxidant when insufficient；
3) material is after the output of gas-liquid separation fixed bed reactors after the completion of reacting, through gas-liquid separator separates material；Its
Middle gas phase returns to the recycling of gas buffer tank as gaseous oxidant, and liquid phase is amine oxide product.
The rate of charge of the PKO, hydrogen peroxide and water determine that the product that general control obtains is dense according to the concentration of products obtained therefrom
Degree is 30~40%；The PKO and active ingredient H in hydrogen peroxide2O2Molar ratio be 1:0.1~1.0；
The PKO, hydrogen peroxide and water are passed through the flows of fixed bed reactors and are determined according to fixed bed reactors dischargeable capacity,
It is 60~120min that general control, which reacts mean residence time,.
The immobilized catalyst being previously added in the fixed bed reactors is that loading type silver catalyst or load type palladium are urged
Agent；The addition of fixed catalyst is passed through the total flow decision of fixed bed reactors according to PKO, hydrogen peroxide and water, generally
Three is passed through the 0.1~1% of the flow per hour of fixed bed reactors；
The gaseous oxidant is ozone, and the ratio of the flow being passed through in fixed bed reactors and PKO flows is 1:10~
100。
A kind of continuous device for preparing fatty alkyl amidopropyl amine oxide, it is characterised in that the device is including the use of pipeline
Liquid material entrance, static mixer, fixed bed reactors, gas-liquid separator, gas buffer tank and the wind turbine being sequentially connected；
The liquid material entrance by accessed respectively by pipeline parallel connection PKO entrances, dioxygen water inlet, distillation water inlet group
At；
The static mixer outlet is connected and fixed a reactor lower end import by pipeline.
The liquid outlet of the gas-liquid separator directly exports liquid product.
The gas buffer tank is equipped with gaseous oxidant entrance, and the outlet of gas buffer tank is connected by being equipped with Air fan pipeline
Connect the import of fixed bed reactors lower end.
The present invention compared with the prior art, has the following advantages：
1) present invention uses continuous production technology, reaction time to be reduced to 1~2 hour from traditional 5~6 hours, greatly
Improve production efficiency greatly.
2) present invention avoids the excessive hydrogen peroxide of common process needs, reduces using ozone, hydrogen peroxide as oxidant
The decomposition of hydrogen peroxide, greatly reduces cost.
3) process units provided by the invention is all configured using existing apparatus, and cost simple in structure is relatively low；This hair
It is bright to realize automation control, to improve product quality and ensure the stability of product quality.
Description of the drawings
Fig. 1 is the system structure diagram of device of the present invention.
In figure：A is PKO entrances, and b is dioxygen water inlet, and c is distillation water inlet, and d is gaseous oxidant entrance, and e is liquid phase
Product；1 is static mixer, and 2 be fixed bed reactors, and 3 be gas-liquid separator, and 4 be gas buffer tank, and 5 be wind turbine.
Specific implementation mode
Below in conjunction with Figure of description, the invention will be further described, but the invention is not limited in following embodiments.
In the continuous device for preparing fatty alkyl amidopropyl amine oxide shown in the drawings：PKO, hydrogen peroxide and distillation
Water (PKO, hydrogen peroxide, distilled water ratio be usually 2~4:1:4~6) anti-into fixed bed after 1 mixing of static mixer
Answer the lower end import of device 2；The oxidant that gasifies is entered the lower end import of fixed bed reactors also by wind turbine 5 by gas buffer tank 4；
The outlet connection gas-liquid separator 3 of fixed bed reactors realizes gas-liquid separation, and the gas after separation returns to gas by pipeline and delays
Tank re-using is rushed, the liquid outlet of gas-liquid separator directly exports liquid product；Gaseous oxidant passes through in gas buffer tank
Pressure detecting, make-up gas oxidant.
Embodiment 1
In effective volume 1.5M3Fixed bed reactors in be added 5000 grams of loading type silver catalyst.
PKO, 27.5% hydrogen peroxide, (weight of material is than 3 for distilled water:1:6) laggard by static mixer with 1000kg/h
Enter fixed bed reactors；It is 0.15Mpa that Maximum Concentration of Ozone is maintained in gas cushion, at the same ozone with the flow velocity of 15kg/h by wind turbine
It delivers into fixed bed reactors.
Fixed bed reactors maintaining reaction temperature is 75 DEG C, the reaction product come out from fixed bed reactors, via gas-liquid
After separation, gas-phase product is collected in gas buffer tank, is continued as gaseous oxidant to reuse, and liquid product is
The fatty alkyl amidopropyl amine oxide (CAO) of target product-a concentration of 31.5%, it is 99.5% to measure conversion ratio.
Embodiment 2
In effective volume 1.5M3Fixed bed reactors in be added 3000 grams of loading type silver catalyst.
PKO, 30% hydrogen peroxide, (weight of material is than 3 for distilled water:1:6) with 1000kg/h by entering after static mixer
Fixed bed reactors；It is 0.2Mpa that Maximum Concentration of Ozone is maintained in gas cushion, while ozone is defeated by wind turbine with the flow velocity of 10kg/h
It is fed into fixed bed reactors.
Fixed bed reactors maintaining reaction temperature is 70 DEG C, the reaction product come out from fixed bed reactors, via gas-liquid
After separation, gas-phase product is collected in gas buffer tank, is continued as gaseous oxidant to reuse, and liquid product is
The fatty alkyl amidopropyl amine oxide (CAO) of target product-a concentration of 31.5%, it is 99.5% to measure conversion ratio.
Claims (5)
1. a kind of method that serialization prepares fatty alkyl amidopropyl amine oxide is carried out according to following steps：
1) fatty acid amide propyl tertiary amine PKO, hydrogen peroxide and water are passed through fixation from bottom after mixing by static mixer
In bed reactor；It is previously added immobilized catalyst in the fixed bed reactors；
2) gaseous oxidant is entered from gas buffer tank in fixed bed reactors by gas transfer pump, with PKO, hydrogen peroxide and gas
Body oxidant is reacted under the action of catalyst in fixed bed reactors, 40~80 DEG C of controlling reaction temperature；Gas buffer tank
Interior gas pressure maintains 0.1~0.5Mpa, by gaseous oxidant entrance make-up gas oxidant when insufficient；
3) material is after the output of gas-liquid separation fixed bed reactors after the completion of reacting, through gas-liquid separator separates material；Wherein gas
The recycling of gas buffer tank mutually is returned to as gaseous oxidant, liquid phase is amine oxide product.
2. the method that serialization according to claim 1 prepares fatty alkyl amidopropyl amine oxide, it is characterised in that：Institute
The rate of charge for stating PKO, hydrogen peroxide and water determines that the product design controlled is 30~40% according to the concentration of products obtained therefrom；
The PKO and active ingredient H in hydrogen peroxide2O2Molar ratio be 1:0.1~1.0；
3. the method that serialization according to claim 1 prepares fatty alkyl amidopropyl amine oxide, it is characterised in that：Institute
It states PKO, hydrogen peroxide and water and is passed through the flows of fixed bed reactors and determined according to fixed bed reactors dischargeable capacity, control reaction is flat
The equal residence time is 60~120min.
4. the method that serialization according to claim 2 or 3 prepares fatty alkyl amidopropyl amine oxide, feature exist
In：The immobilized catalyst being previously added in the fixed bed reactors be loading type silver catalyst or load type palladium catalyst,
The addition of fixed catalyst is PKO, hydrogen peroxide and hydration count the 0.1~1% of the flow per hour for being passed through fixed bed reactors.
5. the method that serialization according to claim 4 prepares fatty alkyl amidopropyl amine oxide, it is characterised in that：Institute
Gaseous oxidant is stated as ozone, the ratio of the flow being passed through in fixed bed reactors and PKO flows is 1:10~100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611244120.1A CN106748897B (en) | 2016-12-29 | 2016-12-29 | A kind of serialization prepares the method and apparatus of fatty alkyl amidopropyl amine oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611244120.1A CN106748897B (en) | 2016-12-29 | 2016-12-29 | A kind of serialization prepares the method and apparatus of fatty alkyl amidopropyl amine oxide |
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| CN106748897A CN106748897A (en) | 2017-05-31 |
| CN106748897B true CN106748897B (en) | 2018-09-07 |
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Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60120848A (en) * | 1983-12-01 | 1985-06-28 | Mitsubishi Petrochem Co Ltd | Preparation of mixed tertiary amine oxide |
| AR065840A1 (en) * | 2007-03-05 | 2009-07-08 | Procter & Gamble | DECOMPOSITION OF HYDROGEN PEROXIDE BY CATALASS IN SURFACTANTS |
| CN106076195B (en) * | 2016-07-28 | 2018-01-09 | 浙江赞宇科技股份有限公司 | A kind of continuous technique and device for preparing alkyl ether carboxylic acid's salt surfactant |
| CN206359448U (en) * | 2016-12-29 | 2017-07-28 | 赞宇科技集团股份有限公司 | A kind of serialization prepares the device of fatty alkyl LAO |
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Address after: Hangzhou City, Zhejiang province 311305 City Shangcheng District No. 128 Lane Applicant after: ZANYU TECHNOLOGY GROUP CO.,LTD. Applicant after: JIAXING ZANYU TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: Qingshan Lake Science and Technology City Xingang Ling'an Road, Hangzhou City, Zhejiang Province, No. 628 311305 Applicant before: ZANYU TECHNOLOGY GROUP CO.,LTD. Applicant before: JIAXING ZANYU TECHNOLOGY DEVELOPMENT Co.,Ltd. |
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Effective date of registration: 20240202 Address after: No. 128 city head lane, Hangzhou, Zhejiang Province Patentee after: ZANYU TECHNOLOGY GROUP CO.,LTD. Country or region after: China Patentee after: JIAXING ZANYU TECHNOLOGY DEVELOPMENT Co.,Ltd. Patentee after: Hangzhou Zanyu Chemical Co.,Ltd. Address before: No. 128, Chengtou lane, Shangcheng District, Hangzhou City, Zhejiang Province Patentee before: ZANYU TECHNOLOGY GROUP CO.,LTD. Country or region before: China Patentee before: JIAXING ZANYU TECHNOLOGY DEVELOPMENT Co.,Ltd. |