CN107118307A - A kind of sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride - Google Patents
A kind of sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride Download PDFInfo
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- CN107118307A CN107118307A CN201710489097.0A CN201710489097A CN107118307A CN 107118307 A CN107118307 A CN 107118307A CN 201710489097 A CN201710489097 A CN 201710489097A CN 107118307 A CN107118307 A CN 107118307A
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- Prior art keywords
- zirconium dichloride
- tetrahydroindenyl zirconium
- functional group
- group containing
- sorbing material
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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
- C08F261/00—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00
- C08F261/02—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols
- C08F261/04—Macromolecular compounds obtained by polymerising monomers on to polymers of oxygen-containing monomers as defined in group C08F16/00 on to polymers of unsaturated alcohols on to polymers of vinyl alcohol
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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
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/32—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
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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
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/08—Vinylidene chloride
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Analytical Chemistry (AREA)
Abstract
The present invention provides a kind of sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride, and its preparation method comprises the following steps：A certain amount of vinylidene chloride is distributed in water, it is proportionally added into cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 2 (allyloxy methyl) 18 are preced with 6 ethers, ammonium persulfate and polyvinyl alcohol, the alcohol phosphate of 9 octadecylene 1,1,3 dicyclohexyls 1,1,3,3 four [(base of ENB 2) ethyl dimethylsilyl bis] disiloxane, the butyl imidazole hexafluorophosphate of 1 vinyl 3, heating, at 90 120 DEG C, react 8 15 hours, product is filtered, drying, that is, obtains the sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, the adsorption material of especially a kind of functional group containing tetrahydroindenyl zirconium dichloride
Material.
Background technology
Expoxy propane, also known as propylene oxide, methyl oxirane, are very important organic compound raw materials, are only secondary
In polypropylene and the third-largest propylene analog derivative of acrylonitrile.Expoxy propane is colourless ether taste liquid, low boiling, inflammable.There is hand
Property, industrial goods are generally the racemic mixture of two kinds of enantiomers.Expoxy propane（PO）It is in addition to polypropylene and acrylonitrile
Three big acryloyl derivatives, are important basic organic chemical industry synthesis materials, mainly for the production of polyethers, propane diols etc..It is also
The primary raw material of forth generation detergent nonionic surfactant, oil field demulsifier, farm chemical emulgent etc..The derivative of expoxy propane
Thing is widely used in the industries such as automobile, building, food, tobacco, medicine and cosmetics.Nearly hundred kinds of the downstream product produced, is essence
Refine the important source material of chemical product.
CN105367520A disclose it is a kind of prepare the method for expoxy propane, including make propylene and cumyl hydroperoxide
The step of reacted logistics is contacted with the logistics containing alkali, removes the trace acidic material generated in epoxidization reaction process,
To reduce product propene oxide and α, decomposition of the alpha-alpha-dimethyl benzylalcohol in subsequent fine cut from during improves expoxy propane and α,
The yield of alpha-alpha-dimethyl benzylalcohol, available in the industrial production of expoxy propane.
CN100400526 discloses a kind of method for purifying expoxy propane, is solvent with methanol, is obtained through epoxidation process
The expoxy propane obtained can be handled by carrying out effective fractionation to crude epoxidation reaction product, to remove acetaldehyde.The fractional distillation process
In, using methanol as solvent to reduce the relative volatility of acetaldehyde impurity, thus the tower of the acetaldehyde containing almost all may be obtained
Bottom effluent.The purified propene oxide of the acetaldehyde containing low concentration is removed as column overhead stream.
Existing sorbing material production method, most adsorption effect is poor, cause product propylene purity have compared with
Big limitation.
The content of the invention
The purpose of the present invention is：There is provided a kind of sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride, it is characterised in that prepare
Step includes：
A certain amount of vinylidene chloride is distributed in water, cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 2- (allyls are added in following ratios
Epoxide methyl) -18- hat 6- ethers, ammonium persulfate and polyvinyl alcohol, 9- octadecene-1-ol phosphates, 1,3- dicyclohexyl -1,1,
3,3- tetra- [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane, 1- vinyl -3- butyl imidazole hexafluorophosphoric acids
Salt, heating, at 90-120 DEG C, is reacted 8-15 hours, and product filtering, drying obtains the suction of the functional group containing tetrahydroindenyl zirconium dichloride
Enclosure material.
Ingredients weight parts
Vinylidene chloride 100
Cyclopentadienyl group tetrahydroindenyl zirconium dichloride 0.01-0.1
2- (allyloxy methyl) -18- hat 6- ethers 0.05-0.15
Ammonium persulfate 1-2
Polyvinyl alcohol 1-2
9- octadecene-1-ol phosphoesterase 30s .01-0.1
1,3- dicyclohexyls -1,1,3,3- four [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane 0.01-0.1
1- vinyl -3- butyl imidazole hexafluorophosphates 0.1-0.5
Water 1000
Described cyclopentadienyl group tetrahydroindenyl zirconium dichloride is commercially available prod, as regent biochemical technology Co., Ltd of Shenzhen produces
Product；2- (allyloxy methyl) -18- hat 6- ethers are commercially available prod, the production of the vast chemical Science and Technology Ltd.'s production of such as Shanghai ancient cooking vessel
Product；9- octadecene-1-ols phosphate is commercially available prod, such as the product of Hangzhou great Yang Chemical Co., Ltd.s production；The hexamethylenes of 1,3- bis-
Base -1,1,3,3- tetra- [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane be commercially available prod, such as Tianjin Skien this
The product of biochemical technology Co., Ltd production；1- vinyl -3- butyl imidazoles hexafluorophosphate is commercially available prod, such as Chinese science
The product of Lanzhou Physical and Chemical Inst. of institute production.
The product of the present invention has the advantages that：
Introduce cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 2- (allyloxy methyl) -18- hat 6- ethers, ammonium persulfate and polyethylene
Alcohol, 9- octadecene-1-ol phosphates, 1,3- dicyclohexyl -1,1,3,3- tetra- [(ENB -2- bases) ethyl dimethyl silicas
Base] disiloxane, 1- vinyl -3- butyl imidazoles hexafluorophosphates are as polymerized monomer, and adsorbent has stronger thermally-stabilised
Property and chemical stability, specific surface area is high, and adsorption rate is fast, and the amount of adsorbing contaminant is big, so the product propylene produced
Purity is higher.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
The addition 100Kg vinylidene chlorides in 2000L reactors, 1000Kg water, 0.05Kg cyclopentadienyl group tetrahydroindenyl zirconium dichlorides,
0.1Kg2- (allyloxy methyl) -18- is preced with 6- ethers, 1.5Kg ammonium persulfates, 1.5Kg polyvinyl alcohol, 0.05Kg9- octadecylenes -1-
Alcohol phosphate, 0.05Kg1,3- dicyclohexyls -1,1,3,3- tetra- [(ENB -2- bases) ethyl dimethylsilyl bis] two silica
Alkane, 0.3Kg1- vinyl -3- butyl imidazole hexafluorophosphates are warming up to 105 DEG C, react 12h, and product filtering, drying is produced
To the sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride.
Embodiment 2
The addition 100Kg vinylidene chlorides in 2000L reactors, 1000Kg water, 0.01Kg cyclopentadienyl group tetrahydroindenyl zirconium dichlorides,
0.05Kg2- (allyloxy methyl) -18- is preced with 6- ethers, 1Kg ammonium persulfates, 1Kg polyvinyl alcohol, 0.01Kg9- octadecene-1-ols
Phosphate, 0.01Kg1,3- dicyclohexyls -1,1,3,3- tetra- [(ENB -2- bases) ethyl dimethylsilyl bis] two silica
Alkane, 0.1Kg1- vinyl -3- butyl imidazole hexafluorophosphates are warming up to 90 DEG C, react 8h, and product filtering, drying obtains
The sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride.
Embodiment 3
The addition 100Kg vinylidene chlorides in 2000L reactors, 1000Kg water, 0.1Kg cyclopentadienyl group tetrahydroindenyl zirconium dichlorides,
0.15Kg2- (allyloxy methyl) -18- is preced with 6- ethers, 2Kg ammonium persulfates, 2Kg polyvinyl alcohol, 0.1Kg9- octadecene-1-ol phosphorus
Acid esters, 0.1Kg1,3- dicyclohexyls -1,1,3,3- tetra- [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane,
0.5Kg1- vinyl -3- butyl imidazole hexafluorophosphates, are warming up to 120 DEG C, react 15h, and product filtering, drying is contained
The sorbing material of tetrahydroindenyl zirconium dichloride functional group.
Comparative example 1
It is added without cyclopentadienyl group tetrahydroindenyl zirconium dichloride, other conditions be the same as Example 1.
Comparative example 2
It is added without 2- (allyloxy methyl) -18- hat 6- ethers, other conditions be the same as Example 1.
Comparative example 3
It is added without 9- octadecene-1-ol phosphates, other conditions be the same as Example 1.
Comparative example 4
It is added without 1,3- dicyclohexyls -1,1,3,3- tetra- [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane, its
His condition be the same as Example 1.
Comparative example 5
It is added without 1- vinyl -3- butyl imidazole hexafluorophosphates, other conditions be the same as Example 1.
Comparative example 6
The adsorbent product that the present invention is produced is added without, is adsorbed with activated carbon.
Embodiment 4
The expoxy propane crude product for being about 85% by mass percent concentration is passed through to be contained equipped with 500g embodiments 1-3 and comparative example 1-6
The 1000L exchange columns of the sorbing material of tetrahydroindenyl zirconium dichloride functional group, temperature 60 C, flow velocity 0.5BV/h, under the conditions of adsorb and carry
It is pure, with the weight/mass percentage composition of gas chromatographic detection efflux, it is shown in Table 1.
Table 1：Product propylene purity after the adsorbent product absorption that different process is produced.
Claims (2)
1. the sorbing material of a kind of functional group containing tetrahydroindenyl zirconium dichloride, it is characterised in that including following material component：
Ingredients weight parts
Vinylidene chloride 100
Cyclopentadienyl group tetrahydroindenyl zirconium dichloride 0.01-0.1
2- (allyloxy methyl) -18- hat 6- ethers 0.05-0.15
Ammonium persulfate 1-2
Polyvinyl alcohol 1-2
9- octadecene-1-ol phosphoesterase 30s .01-0.1
1,3- dicyclohexyls -1,1,3,3- four [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane 0.01-0.1
1- vinyl -3- butyl imidazole hexafluorophosphates 0.1-0.5
Water 1000.
2. the preparation method of the sorbing material of a kind of functional group containing tetrahydroindenyl zirconium dichloride, it is characterised in that comprise the following steps：
A certain amount of vinylidene chloride is distributed in water, cyclopentadienyl group tetrahydroindenyl zirconium dichloride, 2- (allyloxys is proportionally added into
Methyl) -18- hat 6- ethers, ammonium persulfate and polyvinyl alcohol, 9- octadecene-1-ol phosphates, 1,3- dicyclohexyl -1,1,3,3-
Four [(ENB -2- bases) ethyl dimethylsilyl bis] disiloxane, 1- vinyl -3- butyl imidazole hexafluorophosphates rise
Temperature, at 90-120 DEG C, reacts 8-15 hours, and product filtering, drying obtains the adsorption material of the functional group containing tetrahydroindenyl zirconium dichloride
Material.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2016106911835 | 2016-08-21 | ||
| CN201610691183.5A CN106268688A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of expoxy propane purification adsorbent |
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| Publication Number | Publication Date |
|---|---|
| CN107118307A true CN107118307A (en) | 2017-09-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610691183.5A Withdrawn CN106268688A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of expoxy propane purification adsorbent |
| CN201710489097.0A Withdrawn CN107118307A (en) | 2016-08-21 | 2017-06-24 | A kind of sorbing material of the functional group containing tetrahydroindenyl zirconium dichloride |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610691183.5A Withdrawn CN106268688A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of expoxy propane purification adsorbent |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422708B (en) * | 2017-08-28 | 2021-03-30 | 中国石油化工股份有限公司 | Ethylene oxide purification process |
| CN108192026A (en) * | 2017-11-23 | 2018-06-22 | 孝感市锐思新材科技有限公司 | A kind of preparation method of propylene oxide purification material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273583A (en) * | 1997-08-08 | 2000-11-15 | 阿科化学技术公司 | Propylene oxide purification |
| CN103752288A (en) * | 2014-01-22 | 2014-04-30 | 王金明 | Preparation method of adsorbent applied to rapamycin separation |
| CN104058370A (en) * | 2014-06-13 | 2014-09-24 | 王金明 | Method for purifying dimethyl dichlorosilane hydrolysis byproduct hydrochloric acid |
| CN105367520A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Method for preparing propylene oxide |
| CN105597711A (en) * | 2016-03-09 | 2016-05-25 | 张玲 | Preparation method of binary acid refined adsorbing material |
-
2016
- 2016-08-21 CN CN201610691183.5A patent/CN106268688A/en not_active Withdrawn
-
2017
- 2017-06-24 CN CN201710489097.0A patent/CN107118307A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273583A (en) * | 1997-08-08 | 2000-11-15 | 阿科化学技术公司 | Propylene oxide purification |
| CN103752288A (en) * | 2014-01-22 | 2014-04-30 | 王金明 | Preparation method of adsorbent applied to rapamycin separation |
| CN104058370A (en) * | 2014-06-13 | 2014-09-24 | 王金明 | Method for purifying dimethyl dichlorosilane hydrolysis byproduct hydrochloric acid |
| CN105367520A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Method for preparing propylene oxide |
| CN105597711A (en) * | 2016-03-09 | 2016-05-25 | 张玲 | Preparation method of binary acid refined adsorbing material |
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| CN106268688A (en) | 2017-01-04 |
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