CN106349077A - Preparation method of adsorbent for purifying trimethylolpropane oleate - Google Patents
Preparation method of adsorbent for purifying trimethylolpropane oleate Download PDFInfo
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- CN106349077A CN106349077A CN201610691181.6A CN201610691181A CN106349077A CN 106349077 A CN106349077 A CN 106349077A CN 201610691181 A CN201610691181 A CN 201610691181A CN 106349077 A CN106349077 A CN 106349077A
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- dimethyl
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/22—Vinylidene fluoride
- C08F214/225—Vinylidene fluoride with non-fluorinated comonomers
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method of an adsorbent for purifying trimethylolpropane oleate. The preparation method includes dispersing a certain amount of vinylidene chloride into water, adding 2-acrylamide-2-methylpropanesulfonic acid, bicyclo[2.2.1]hept-5-ene-2-carboxylic acid tert-butyl ester, ammonium persulfate, polyvinyl alcohol, 1,1-bis(trimethylsilyloxy)-3,3-dimethyl-1-butene,(cyclopentadienyl)(1,3-dimethylcyclopentadienyl)zirconium dichloride and 1-vinyl-3-butylimidazolium bis(trifluoromethylsulfonyl)imide according to a specific proportion, increasing the temperature, reacting at a suitable temperature and filtering and drying a product so as to obtain the adsorbent for purifying the trimethylolpropane oleate.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of tricarboxymethyl propane oleate purification absorption
The preparation method of agent.
Background technology
Tricarboxymethyl propane oleate, has good greasy property, and biological degradation rate is very high, and viscosity index (VI) is high, resists
Combustion property is good, is No. 46 synthesis preferable base oils of ester type fire resistant hydraulic oil；Can be used for hydraulic oil, the chain saw oil of formulation requirements environmental protection
Disable engine oil with trip waterborne；As oiliness improver cold-rolling of steel plate liquid, steel plate drawing oil, cutting oil, releasing agent and other
Widely use in metal working fluid.Also can be used as the intermediate of leather auxiliary agent and textile finish oil.
Cn104387271a discloses a kind of cyclic regeneration absorption purifying technique of tricarboxymethyl propane oleate, technique
Operating procedure is: (1) loads adsorbent in the adsorption tower of one or more series connection；(2) tricarboxymethyl propane oleate crude product exists
The adsorption tower being filled with adsorbent is continued through, wherein impact product non-oxidizability and emulsion resistance under certain flow rate and uniform temperature
Property impurity, such as minute solid particles, colloid etc. be adsorbed by adsorbent；(3) the cyclic regeneration of adsorbent: washed with low-carbon alcohols circulation
Wash, to remove the organic impuritiess such as adsorbent colloid, then with inert gas purge, be vacuum dried regeneration, the suction after regeneration
Can reuse for attached dose.
Cn1379014 discloses a kind of synthetic method of tricarboxymethyl propane oleate, belongs to esters chemical combination in organic chemistry
The synthesis technical field of thing, with trimethylolpropane and Oleic acid as raw material it is characterised in that adding in soild oxide and binary acid
Plus carry out dehydration condensation in the presence of agent, add water stirring and be hydrolyzed reaction, then in the fine vacuum bar of 20～100pa
Carry out high-temperature process under part and tricarboxymethyl propane oleate is obtained, the addition of soild oxide and binary acid additive is respectively
Trimethylolpropane and the 0.1～0.8% and 2～10% of Oleic acid gross weight.Described additive can be decanedioic acid, adipic acid, ten
The mixture of any one or more of two carbon diacid etc..
Existing tricarboxymethyl propane oleate produces or method of purification, does not mostly adopt the adsorbent of adsorbent or employing
Adsorption effect is poor, needs repeatedly to adsorb often, leads to the purity of tricarboxymethyl propane oleate product to have compared with the day of one's doom
System.
Content of the invention
The purpose of the present invention is: provides a kind of preparation method of tricarboxymethyl propane oleate purification adsorbent, it can
To be applied in tricarboxymethyl propane oleate purification, its adsorption rate is fast, and adsorbing contaminant amount is big, so applying this absorption
The tricarboxymethyl propane oleate product purity that agent produces is high.It is characterized in that preparation process includes:
A certain amount of vinylidene chloride is distributed in water, adds 2- acrylamide base -2- methyl propane sulfonic acid in following ratios, bicyclic
Double (the trimethylsiloxy) -3,3- of [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester, Ammonium persulfate. and polyvinyl alcohol, 1,1-
Dimethyl -1-butylene, (cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride, 1- vinyl -3- 1-Butyl-1H-imidazole
Double trifluoromethanesulfonimide salt, heat up, and at 80-110 DEG C, react 6-14 hour, product filters, dry, that is, obtain three hydroxyl first
Base propane oleate purification adsorbent.
Ingredients weight parts
Vinylidene chloride 100
2- acrylamide base -2- methyl propane sulfonic acid 0.01-0.1
Bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester 0.05-0.15
Ammonium persulfate. 2-3
Polyvinyl alcohol 1-2
Double (the trimethylsiloxy) -3,3- dimethyl -1-butylene 0.01-0.1 of 1,1-
(cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride 0.01-0.1
The double trifluoromethanesulfonimide salt 0.1-0.5 of 1- vinyl -3- 1-Butyl-1H-imidazole
Water 1000
Described 2- acrylamide base -2- methyl propane sulfonic acid is commercially available prod, and such as Shanghai one is ground bio tech ltd and produced
Product；Bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester is commercially available prod, and such as Shen Feng Chemical Co., Ltd. of Taixing City produces
Product；1,1- double (trimethylsiloxy) -3,3- dimethyl -1-butylene are commercially available prod, and such as Shenzhen's regent is biochemical
The product that Science and Technology Ltd. produces；(cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride is commercially available prod,
The product producing as Alpha Chemical Co., Ltd.；The double trifluoromethanesulfonimide salt of 1- vinyl -3- 1-Butyl-1H-imidazole is commercially available
Product, the product that such as Lanzhou Physical and Chemical Inst. of the Chinese Academy of Sciences produces.
The product of the present invention has the advantages that
Introduce the double trifluoromethanesulfonimide salt of 1- vinyl -3- 1-Butyl-1H-imidazole, 1,1- double (trimethylsiloxy) -3,
3- dimethyl -1-butylene, (cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride, 2- acrylamide base -2- first
As polymerized monomer, adsorbent has higher heat stability and chemical stability to base propane sulfonic acid, and specific surface area is high, adsorption rate
Hurry up, the amount of adsorbing contaminant is big, so the tricarboxymethyl propane oleate product purity produced is higher.
Specific embodiment
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
100kg vinylidene chloride, 1000kg water, 0.05kg2- acrylamide base -2- methyl-prop sulphur is added in 2000l reactor
Acid, 0.1kg bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester, 2.5kg Ammonium persulfate., 1.5kg polyvinyl alcohol, 0.05kg1,
Double (trimethylsiloxy) -3,3- dimethyl -1-butylene of 1-, 0.05kg (cyclopentano diene) (1,3- dimethyl cyclopentano
Diene) zirconium dichloride, the double trifluoromethanesulfonimide salt of 0.3kg1- vinyl -3- 1-Butyl-1H-imidazole, it is warming up to 95 DEG C, reaction
10h, product filters, and dries, that is, obtains tricarboxymethyl propane oleate purification adsorbent.
Embodiment 2
100kg vinylidene chloride, 1000kg water, 0.01kg2- acrylamide base -2- methyl-prop sulphur is added in 2000l reactor
Acid, 0.05kg bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester, 2kg Ammonium persulfate., 1kg polyvinyl alcohol, 0.01kg1,1- are double
(trimethylsiloxy) -3,3- dimethyl -1-butylene, 0.01kg (cyclopentano diene) (1,3- dimethyl cyclopentano diene)
Zirconium dichloride, the double trifluoromethanesulfonimide salt of 0.1kg1- vinyl -3- 1-Butyl-1H-imidazole, it is warming up to 80 DEG C, react 6h, product
Filter, dry, that is, obtain tricarboxymethyl propane oleate purification adsorbent.
Embodiment 3
Addition 100kg vinylidene chloride in 2000l reactor, 1000kg water, 0.1kg2- acrylamide base -2- methyl propane sulfonic acid,
0.15kg bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester, 3kg Ammonium persulfate., 2kg polyvinyl alcohol, 0.1kg1,1- double (three
Methyl silicane epoxide) -3,3- dimethyl -1-butylene, 0.1kg (cyclopentano diene) (1,3- dimethyl cyclopentano diene) dichloro
Change zirconium, the double trifluoromethanesulfonimide salt of 0.5kg1- vinyl -3- 1-Butyl-1H-imidazole, it is warming up to 110 DEG C, react 14h, product mistake
Filter, dries, that is, obtains tricarboxymethyl propane oleate purification adsorbent.
Comparative example 1
It is added without 2- acrylamide base -2- methyl propane sulfonic acid, other conditions are with embodiment 1.
Comparative example 2
It is added without bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester, other conditions are with embodiment 1.
Comparative example 3
It is added without double (trimethylsiloxy) -3,3- dimethyl -1-butylene of 1,1-, other conditions are with embodiment 1.
Comparative example 4
It is added without (cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride, other conditions are with embodiment 1.
Comparative example 5
It is added without the double trifluoromethanesulfonimide salt of 1- vinyl -3- 1-Butyl-1H-imidazole, other conditions are with embodiment 1.
Comparative example 6
It is added without the adsorbent product that the present invention is produced, adsorbed with activated carbon.
Embodiment 4
The tricarboxymethyl propane oleate crude product that mass percent concentration is about 95% be passed through equipped with 500g embodiment 1-3 and
The 1000l exchange column of comparative example 1-6 adsorbent product, 80 DEG C of temperature, flow velocity 0.5bv/h, under the conditions of absorption purification, use gas phase color
The weight/mass percentage composition of spectrum detection effluent, is shown in Table 1.
Table 1: the tricarboxymethyl propane oleate product purity after the adsorbent product absorption that different process is produced.
| Numbering | Tricarboxymethyl propane oleate purity (%) |
| Embodiment 1 | 99.4 |
| Embodiment 2 | 99.4 |
| Embodiment 3 | 99.8 |
| Comparative example 1 | 97.9 |
| Comparative example 2 | 98.0 |
| Comparative example 3 | 97.5 |
| Comparative example 4 | 97.8 |
| Comparative example 5 | 97.7 |
| Comparative example 6 | 96.8 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with the present invention it is
Basis, for solving essentially identical technical problem, realizes essentially identical technique effect, done simple change, equivalent replaces
Change or modify, be all covered by among protection scope of the present invention.
Claims (2)
1. a kind of tricarboxymethyl propane oleate purification adsorbent is it is characterised in that include following material component:
Ingredients weight parts
Vinylidene chloride 100
2- acrylamide base -2- methyl propane sulfonic acid 0.01-0.1
Bicyclic [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester 0.05-0.15
Ammonium persulfate. 2-3
Polyvinyl alcohol 1-2
Double (the trimethylsiloxy) -3,3- dimethyl -1-butylene 0.01-0.1 of 1,1-
(cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride 0.01-0.1
The double trifluoromethanesulfonimide salt 0.1-0.5 of 1- vinyl -3- 1-Butyl-1H-imidazole
Water 1000.
2. a kind of preparation method of tricarboxymethyl propane oleate purification adsorbent is it is characterised in that comprise the following steps:
A certain amount of vinylidene chloride is distributed in water, is proportionally added into 2- acrylamide base -2- methyl propane sulfonic acid, bicyclic
Double (the trimethylsiloxy) -3,3- of [2.2.1] hept- 5- alkene -2- carboxylic acid tert-butyl ester, Ammonium persulfate. and polyvinyl alcohol, 1,1-
Dimethyl -1-butylene, (cyclopentano diene) (1,3- dimethyl cyclopentano diene) zirconium dichloride, 1- vinyl -3- 1-Butyl-1H-imidazole
Double trifluoromethanesulfonimide salt, heat up, and at 80-110 DEG C, react 6-14 hour, product filters, dry, that is, obtain three hydroxyl first
Base propane oleate purification adsorbent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691181.6A CN106349077A (en) | 2016-08-21 | 2016-08-21 | Preparation method of adsorbent for purifying trimethylolpropane oleate |
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| CN201610691181.6A CN106349077A (en) | 2016-08-21 | 2016-08-21 | Preparation method of adsorbent for purifying trimethylolpropane oleate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387271A (en) * | 2014-10-30 | 2015-03-04 | 南京威尔化工有限公司 | Continuous regeneration adsorption purification process of trimethylolpropane trioleate |
| CN105833854A (en) * | 2016-06-13 | 2016-08-10 | 王金明 | Preparation method of purified vanadium adsorption material |
| CN105859938A (en) * | 2016-06-13 | 2016-08-17 | 王金明 | Preparation of cobalt adsorbent |
-
2016
- 2016-08-21 CN CN201610691181.6A patent/CN106349077A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104387271A (en) * | 2014-10-30 | 2015-03-04 | 南京威尔化工有限公司 | Continuous regeneration adsorption purification process of trimethylolpropane trioleate |
| CN105833854A (en) * | 2016-06-13 | 2016-08-10 | 王金明 | Preparation method of purified vanadium adsorption material |
| CN105859938A (en) * | 2016-06-13 | 2016-08-17 | 王金明 | Preparation of cobalt adsorbent |
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Address after: 432000 Hubei city of Xiaogan province high tech Zone Qun Sheng Cun Nan Qu Bian min Lu 5 floor, room 91 Applicant after: Wang Qiyu Address before: 432000 Hubei city of Xiaogan province high tech Zone Danyang District Community Lisi mall two Room 201 Applicant before: Wang Qiyu |
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Address after: The new school district 322009 town Zhejiang city Yiwu province 5 Building 1 unit 201 room Applicant after: Wang Qiyu Address before: 432000 Hubei city of Xiaogan province high tech Zone Qun Sheng Cun Nan Qu Bian min Lu 5 floor, room 91 Applicant before: Wang Qiyu |
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Application publication date: 20170125 |