CN106311150A - Preparation method of adsorbent for purification of trimethylolpropane trioleate - Google Patents
Preparation method of adsorbent for purification of trimethylolpropane trioleate Download PDFInfo
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- CN106311150A CN106311150A CN201610691207.7A CN201610691207A CN106311150A CN 106311150 A CN106311150 A CN 106311150A CN 201610691207 A CN201610691207 A CN 201610691207A CN 106311150 A CN106311150 A CN 106311150A
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- Prior art keywords
- adsorbent
- purification
- propane oleate
- tricarboxymethyl propane
- mnb
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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
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
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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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a preparation method of an adsorbent for purification of trimethylolpropane trioleate. The method comprises the following steps: dispersing a certain amount of styrene to water, proportionally adding 5-methylene-norbornene (MNB), 2-ethylhexyl vinyl ether, pentamethylcyclopentadienyl titanium trimethyl, potassium persulfate and sodium dodecyl benzene sulfonate and 2-methyl vinyl butyrate, raising the temperature, enabling reaction at appropriate temperature, filtering and drying the product to obtain the adsorbent for purifying trimethylolpropane trioleate.
Description
Technical field
The present invention relates to the preparation method of a kind of adsorbent, especially a kind of tricarboxymethyl propane oleate purification absorption
The preparation method of agent.
Background technology
It is high that tricarboxymethyl propane oleate has viscosity index (VI), and flame resistance is good, the feature of excellent lubricating properties, and has
The highest biological degradation rate.It is No. 46 synthesis preferable base oils of ester type fire resistant hydraulic oil；Can be used for formulation requirements environmental protection
Hydraulic oil, chain saw oil and water ride engine oil；As oiliness improver cold-rolling of steel plate liquid, steel pipe drawing oil, cutting oil,
It is widely used in releasing agent and other metal working fluid.Also can be as the intermediate of leather auxiliary agent and textile finish oil.High-purity
The tricarboxymethyl propane oleate of degree has more excellent stability and lubricity.
CN104387271A discloses the cyclic regeneration absorption purifying technique of a kind of tricarboxymethyl propane oleate, technique
Operating procedure is: (1) loaded by adsorbent in the adsorption tower of one or more series connection；(2) tricarboxymethyl propane oleate crude product exists
Continue through the adsorption tower being filled with adsorbent under certain flow rate and uniform temperature, wherein affect product non-oxidizability and emulsion resistance
The impurity of property, as minute solid particles, colloid etc. are adsorbed by adsorbent；(3) the cyclic regeneration of adsorbent: wash with low-carbon alcohols circulation
Wash, to remove the organic impuritiess such as adsorbent colloid, then by inert gas purge, be vacuum dried regeneration, the suction after regeneration
Can reuse for attached dose.
CN102010332A disclose a kind of solid superacid as catalyst produce tricarboxymethyl propane oleate method and
Application.It is made up of following step: esterification: trimethylolpropane and oleic acid in mass ratio 1: 2.1-9.5 are mixed, adds simultaneously
Entering solid super-strong acid, under 10-1000Pa vacuum, 120-200 DEG C is reacted 4-10 hour;Filter: use 10-600 mesh filter screen
Or filter plate, product is filtered, removes solid super-strong acid;Remove unreacted reactant: the product after filtration is heated to
180-300 DEG C, system vacuum is maintained at 1-1000Pa, and decompression distillation removes unreacted reactant in 40-120 minute, obtains three
Hydroxymethyl-propane oleate.
Existing purification tricarboxymethyl propane oleate technology, has operation complex, and adsorption rate is slow, produces
The shortcoming that tricarboxymethyl propane oleate purity is not high enough.
Summary of the invention
It is an object of the invention to: providing the preparation method of a kind of tricarboxymethyl propane oleate purification adsorbent, it can
To be applied to produce in tricarboxymethyl propane oleate, application is simple, and adsorption rate is fast, and the trimethylolpropane oil produced
Acid esters purity is high.It is characterized in that preparation process includes:
A certain amount of styrene is distributed in water, adds 5-methylene-2-norbornene (MNB), 2-ethyl in following ratio
Hexyl vinyl ethers, pentamethylcyclopentadiene base titanium trimethyl, potassium peroxydisulfate and dodecylbenzene sodium sulfonate, 2-Methyl Butyric Acid
Vinyl acetate, heats up, at 80-110 DEG C, reacts 6-15 hour, and product filters, and dries, i.e. obtains tricarboxymethyl propane oleate and carry
Pure adsorbent.
Ingredients weight parts
Styrene 100
5-methylene-2-norbornene (MNB) monomer 5-15
2-ethylhexyl vinyl ether 1-5
Potassium peroxydisulfate 0.2-0.8
Dodecylbenzene sodium sulfonate 0.5-1.5
2-Methyl Butyric Acid vinyl acetate 0.1-1
Pentamethylcyclopentadiene base titanium trimethyl 0.1-0.5
Water 1000
Described 5-methylene-2-norbornene (MNB) monomer is commercially available prod, as Puyang Hui Cheng Electron Material Co., Ltd produces
Product；2-ethylhexyl vinyl ether is commercially available prod, the product produced such as Hubei Xinjing New Material Co., Ltd.；Dodecane
Base benzene sulfonic acid sodium salt is commercially available prod, the product produced such as Shanghai Yan Sheng Science and Technology Ltd.；2-Methyl Butyric Acid vinyl acetate is commercially available
Product, the product produced such as Hubei Ju Sheng Science and Technology Ltd.；Pentamethylcyclopentadiene base titanium trimethyl is commercially available prod, such as Hangzhoupro
The product that Zhou great Yang Chemical Co., Ltd. produces.
The product of the present invention has the advantages that
It is big that the adsorbent product produced by this technique has specific surface area, and adsorption rate is fast, the advantage that adsorbing contaminant amount is big,
When actual production tricarboxymethyl propane oleate, it is easy and simple to handle that absorption purifies link, the trimethylolpropane oleic acid produced
Ester product purity is high.
Detailed description of the invention
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
In 2000L reactor, adding 1000Kg water, 100Kg styrene, 10Kg5-methylene-2-norborene (MNB) is single
Body, 3Kg2-ethylhexyl vinyl ether, 0.5Kg potassium peroxydisulfate, 1Kg dodecylbenzene sodium sulfonate, 0.5Kg2-methylbutanoic acid second
Alkene ester, 0.3Kg pentamethylcyclopentadiene base titanium trimethyl, stir, be warming up to 100 DEG C, react 10h, product, through filtering, dries
Do and i.e. obtain tricarboxymethyl propane oleate purification adsorbent.
Embodiment 2
In 2000L reactor, addition 1000Kg water, 100Kg styrene, 5Kg5-methylene-2-norborene (MNB) monomer,
1Kg2-ethylhexyl vinyl ether, 0.2Kg potassium peroxydisulfate, 0.5Kg dodecylbenzene sodium sulfonate, 0.1Kg2-methylbutanoic acid ethylene
Ester, 0.1Kg pentamethylcyclopentadiene base titanium trimethyl, stir, be warming up to 80 DEG C, react 6h, product, through filtering, is dried i.e.
Obtain tricarboxymethyl propane oleate purification adsorbent.
Embodiment 3
In 2000L reactor, adding 1000Kg water, 100Kg styrene, 15Kg5-methylene-2-norborene (MNB) is single
Body, 5Kg2-ethylhexyl vinyl ether, 0.8Kg potassium peroxydisulfate, 1.5Kg dodecylbenzene sodium sulfonate, 1Kg2-methylbutanoic acid second
Alkene ester, 0.5Kg pentamethylcyclopentadiene base titanium trimethyl, stir, be warming up to 110 DEG C, react 15h, product, through filtering, dries
Do and i.e. obtain tricarboxymethyl propane oleate purification adsorbent.
Comparative example 1
Being added without 2-ethylhexyl vinyl ether, other conditions are with embodiment 1.
Comparative example 2
Being added without 2-Methyl Butyric Acid vinyl acetate, other conditions are with embodiment 1.
Comparative example 3
Being added without pentamethylcyclopentadiene base titanium trimethyl, other conditions are with embodiment 1.
Comparative example 4
Not using the adsorbent product that the present invention provides, applied activated carbon adsorbs.
Embodiment 4
By the tricarboxymethyl propane oleate crude product that 500g weight/mass percentage composition is 97%, be passed through equipped with this patent embodiment 1-3 with
And in 1000 exchange columns of adsorbent 500g prepared of comparative example 1-4, flow velocity 1BV/h, temperature 60 C, use gas chromatographic detection stream
Going out the weight/mass percentage composition of liquid, purity is shown in Table 1.
Table 1: trimethylolpropane oil product purity after the adsorbent purification that different process is produced
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, it is achieved essentially identical technique effect, done simple change, equivalent are replaced
Change or modification etc., be all covered by among protection scope of the present invention.
Claims (2)
1. the preparation method of a tricarboxymethyl propane oleate purification adsorbent, it is characterised in that comprise the following steps:
A certain amount of styrene is distributed in water, is proportionally added into 5-methylene-2-norbornene (MNB), 2-ethylhexyl
Vinyl ethers, pentamethylcyclopentadiene base titanium trimethyl, potassium peroxydisulfate and dodecylbenzene sodium sulfonate, 2-Methyl Butyric Acid ethylene
Ester, heats up, at 80-110 DEG C, reacts 6-15 hour, and product filters, and dries, and i.e. obtains tricarboxymethyl propane oleate and purifies use
Adsorbent.
Tricarboxymethyl propane oleate purification adsorbent the most according to claim 1, it is characterised in that: raw material components
Ratio is styrene 100 parts, 5-methylene-2-norbornene (MNB) monomer 5-15 part, 2-ethylhexyl vinyl by weight
Base ether 1-5 part, potassium peroxydisulfate 0.2-0.8 part, dodecylbenzene sodium sulfonate 0.5-1.5,2-Methyl Butyric Acid vinyl acetate 0.1-1 part,
Pentamethylcyclopentadiene base titanium trimethyl 0.1-0.5 part, 1000 parts of water.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691207.7A CN106311150A (en) | 2016-08-21 | 2016-08-21 | Preparation method of adsorbent for purification of trimethylolpropane trioleate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610691207.7A CN106311150A (en) | 2016-08-21 | 2016-08-21 | Preparation method of adsorbent for purification of trimethylolpropane trioleate |
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| CN201610691207.7A Pending CN106311150A (en) | 2016-08-21 | 2016-08-21 | Preparation method of adsorbent for purification of trimethylolpropane trioleate |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340066A (en) * | 1999-02-19 | 2002-03-13 | 拜尔公司 | Polymers based on vinylcyclohexane |
| CN105294910A (en) * | 2015-11-30 | 2016-02-03 | 王金明 | Preparation method of sorbent applied to pristinamycin separation |
| 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 CN201610691207.7A patent/CN106311150A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1340066A (en) * | 1999-02-19 | 2002-03-13 | 拜尔公司 | Polymers based on vinylcyclohexane |
| CN105294910A (en) * | 2015-11-30 | 2016-02-03 | 王金明 | Preparation method of sorbent applied to pristinamycin separation |
| 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: The new school district 322009 town Zhejiang city Yiwu province 5 Building 1 unit 201 room Applicant after: Wang Jinzhen Address before: 315042 Zhejiang province Jiangdong District of Ningbo City Road 265 Lane 17 No. 104 Min'an room Applicant before: Wang Jinzhen |
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Application publication date: 20170111 |