CN108295821A - A kind of preparation method of tricarboxymethyl propane oleate purified material - Google Patents
A kind of preparation method of tricarboxymethyl propane oleate purified material Download PDFInfo
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- CN108295821A CN108295821A CN201711262956.9A CN201711262956A CN108295821A CN 108295821 A CN108295821 A CN 108295821A CN 201711262956 A CN201711262956 A CN 201711262956A CN 108295821 A CN108295821 A CN 108295821A
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- purified material
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- tricarboxymethyl propane
- propane oleate
- graphene sponge
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0259—Compounds of N, P, As, Sb, Bi
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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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/22—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
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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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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Abstract
The present invention relates to a kind of preparation methods of tricarboxymethyl propane oleate purified material.By weight, graphene sponge, acrylate, diallyl diethoxy silane are added in a kettle, 23,4 epoxy of chlorine, 1 butylene, 2 methyl, 2 acrylic acid, 2 butoxyethyl, 1,3,5 benzene tricarbonic acid's triallyls, 3 ethyl-acetylene base trimethyl silane of furans, ammonium persulfate, water, polyvinyl alcohol, heating, reaction, product is through filtering after reaction, washing, it is dry to get to tricarboxymethyl propane oleate purified material.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of tricarboxymethyl propane oleate purified material
Preparation method.
Background technology
Tricarboxymethyl propane oleate has that excellent greasy property, viscosity index (VI) are high, flame resistance is good, hydrolytic stability
Good, high-flash, low volatilization, low-temperature characteristics are good.It is No. 46 synthesis ideal base oils of ester type fire resistant hydraulic oil；It can be used for allocating and want
Ask hydraulic oil, chain saw oil and the water ride engine oil of environmental protection；As oiliness improver in cold-rolling of steel plate liquid, steel pipe drawing oil
And it is widely used in other metal working fluids；Also the intermediate and textile finish oil of leather auxiliary agent be can be used as.
CN106117051A discloses a kind of preparation method of the high-purity oleate of trimethylolpropane, belongs to green technology
Field.The present invention provides a kind of preparation method of the high-purity oleate of trimethylolpropane, the present invention uses collosol and gel legal system
The solid super-strong acid of standby molecular sieve load sulfuric acid/titanium dioxide, to be catalyzed the esterification of trimethylolpropane and high-purity oleic acid,
The biodegradable high-purity oleate of trimethylolpropane is made,
CN1245372 discloses a kind of synthetic method of tricarboxymethyl propane oleate, belongs to ester type compound in organic chemistry
Synthesis technical field, using trimethylolpropane and oleic acid as raw material, it is characterised in that in soild oxide and binary acid additive
Under the action of carry out dehydration condensation, add water stirring and reaction be hydrolyzed, then under the high vacuum condition of 20~100Pa
The addition of the obtained tricarboxymethyl propane oleate of progress high-temperature process, soild oxide and binary acid additive is respectively three hydroxyls
The 0.1~0.8% and 2~10% of methylpropane and oleic acid total weight.The additive can be decanedioic acid, adipic acid, 12
Any one or more mixtures of carbon diacid etc..
Existing tricarboxymethyl propane oleate obtains preparation process, and the process is more complicated for purification link, when having consumption
Between it is long, consume energy more than disadvantage.A kind of novel tricarboxymethyl propane oleate purification adsorbent is researched and developed, purification can be shortened
The time loss of technique, and simplify technique.
Invention content
The purpose of the present invention is：A kind of preparation method of tricarboxymethyl propane oleate purified material is provided, feature exists
Include in preparation process：
By weight, it is added graphene sponge in a kettle, acrylate, diallyl diethoxy silane, 2- chloro- 3,
4- epoxy-1-butylenes, 2- methyl -2- acrylic acid -2- butoxyethyls, 1,3,5- benzene tricarbonic acid's triallyl, furans -3- base second
Alkynyl trimethyl silane, ammonium persulfate, water, polyvinyl alcohol are warming up to 80-90 DEG C, react 10-18h, and product passes through after reaction
Filtering, washing are dry to get to tricarboxymethyl propane oleate purified material.
The acrylate, quality dosage are the 10-20% of graphene sponge.
The diallyl diethoxy silane, quality dosage are the 1-5% of graphene sponge.
Chloro- 3, the 4- epoxy-1-butylenes of the 2-, quality dosage are the 1-5% of graphene sponge.
2- methyl -2- acrylic acid -2- the butoxyethyls, quality dosage are the 1-5% of graphene sponge.
Described 1,3,5- benzene tricarbonic acid's triallyls, quality dosage are the 0.1-0.5% of graphene sponge.
Furans -3- ethyl-acetylene base the trimethyl silanes, quality dosage are the 0.5-1.5% of graphene sponge.
The ammonium persulfate, quality dosage are the 0.5-2% of graphene sponge.
The water, quality dosage are the 400-800% of graphene sponge.
The polyvinyl alcohol, quality dosage are the 0.5-1.5% of graphene sponge.
The graphene sponge, acrylate, diallyl diethoxy silane, chloro- 3, the 4- epoxy-1-butylenes of 2-,
2- methyl -2- acrylic acid -2- butoxyethyls, 1,3,5- benzene tricarbonic acid's triallyl, furans -3- ethyl-acetylene base trimethyl silicanes
Alkane, ammonium persulfate, polyvinyl alcohol are commercial product.
The product of the present invention has the advantages that：
There is character to stablize, the advantages of being easily isolated, compare table for the tricarboxymethyl propane oleate purified material that the present invention is produced
Area is big, and adsorption capacity is big, there is certain specific aim for impurity present in tricarboxymethyl propane oleate, is applied to three hydroxyls
Oleate purifies link, can produce the tricarboxymethyl propane oleate of high-purity.
Specific implementation mode
Following instance is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
Embodiment 1
In a kettle, graphene sponge 100Kg, acrylate 15Kg, diallyl diethoxy silane 1.5Kg, 2- is added
Chloro- 3,4- epoxy-1-butylenes 1.5Kg, 2- methyl -2- acrylic acid -2- butoxyethyls 2Kg, 1,3,5- benzene tricarbonic acid, three allyl
Ester 0.2Kg, furans -3- ethyl-acetylene base trimethyl silane 1Kg, ammonium persulfate 0.75Kg, water 600Kg, polyvinyl alcohol 1Kg, heating
To 90 DEG C, 14h is reacted, for product through filtering, washing is dry to purify material to get to tricarboxymethyl propane oleate after reaction
Material.
Embodiment 2
In a kettle, graphene sponge 100Kg is added, acrylate 10Kg, diallyl diethoxy silane 1Kg, 2- are chloro-
3,4- epoxy-1-butylene 1Kg, 2- methyl -2- acrylic acid -2- butoxyethyls 1Kg, 1,3,5- benzene tricarbonic acid's triallyl
0.1Kg, furans -3- ethyl-acetylene base trimethyl silane 0.5Kg, ammonium persulfate 0.5Kg, water 400Kg, polyvinyl alcohol 0.5Kg, heating
To 80 DEG C, 10h is reacted, for product through filtering, washing is dry to purify material to get to tricarboxymethyl propane oleate after reaction
Material.
Embodiment 3
In a kettle, graphene sponge 100Kg is added, acrylate 20Kg, diallyl diethoxy silane 5Kg, 2- are chloro-
3,4- epoxy-1-butylene 5Kg, 2- methyl -2- acrylic acid -2- butoxyethyls 5Kg, 1,3,5- benzene tricarbonic acid's triallyl
0.5Kg, furans -3- ethyl-acetylene bases trimethyl silane 1.5Kg, ammonium persulfate 2Kg, water 800Kg, polyvinyl alcohol 1.5Kg are warming up to
100 DEG C, 18h is reacted, for product through filtering, washing is dry to purify material to get to tricarboxymethyl propane oleate after reaction
Material.
Comparative example 1
It is added without diallyl diethoxy silane, other conditions are the same as embodiment 1.
Comparative example 2
Chloro- 3, the 4- epoxy-1-butylenes of 2- are added without, other conditions are the same as embodiment 1.
Comparative example 3
2- methyl -2- acrylic acid -2- butoxyethyls are added without, other conditions are the same as embodiment 1.
Comparative example 4
1,3,5- benzene tricarbonic acid's triallyls are added without, other conditions are the same as embodiment 1.
Comparative example 5
Furans -3- ethyl-acetylene base trimethyl silanes are added without, other conditions are the same as embodiment 1.
Embodiment 4
The tricarboxymethyl propane oleate crude product for being about 97% by 500g mass percentages is passed through equipped with this patent embodiment 1-3
And in 1000 exchange columns of the adsorbent 500g of comparative example 1-5 preparations, flow velocity 0.5BV/h, temperature 70 C is examined with gas-chromatography
The mass percentage of efflux is surveyed, purity is shown in Table 1.
Table 1：Trimethylolpropane oil product purity after the adsorbent absorption purification that different process is produced.
Claims (10)
1. a kind of preparation method of tricarboxymethyl propane oleate purified material, it is characterised in that include the following steps：
By weight, it is added graphene sponge in a kettle, acrylate, diallyl diethoxy silane, 2- chloro- 3,
4- epoxy-1-butylenes, 2- methyl -2- acrylic acid -2- butoxyethyls, 1,3,5- benzene tricarbonic acid's triallyl, furans -3- base second
Alkynyl trimethyl silane, ammonium persulfate, water, polyvinyl alcohol are warming up to 80-100 DEG C, react 10-18h, after reaction product
Through filtering, washing is dry to get to tricarboxymethyl propane oleate purified material.
2. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
The acrylate, quality dosage are the 10-20% of graphene sponge.
3. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
The diallyl diethoxy silane, quality dosage are the 1-5% of graphene sponge.
4. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
Chloro- 3, the 4- epoxy-1-butylenes of the 2-, quality dosage are the 1-5% of graphene sponge.
5. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
2- methyl -2- acrylic acid -2- the butoxyethyls, quality dosage are the 1-5% of graphene sponge.
6. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
Described 1,3,5- benzene tricarbonic acid's triallyls, quality dosage are the 0.1-0.5% of graphene sponge.
7. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
Furans -3- ethyl-acetylene base the trimethyl silanes, quality dosage are the 0.5-1.5% of graphene sponge.
8. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
The ammonium persulfate, quality dosage are the 0.5-5% of graphene sponge.
9. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, it is characterised in that：
The water, quality dosage are the 400-800% of graphene sponge.
10. a kind of preparation method of tricarboxymethyl propane oleate purified material according to claim 1, feature exist
In：The polyvinyl alcohol, quality dosage are the 0.5-1.5% of graphene sponge.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711262956.9A CN108295821A (en) | 2017-12-04 | 2017-12-04 | A kind of preparation method of tricarboxymethyl propane oleate purified material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711262956.9A CN108295821A (en) | 2017-12-04 | 2017-12-04 | A kind of preparation method of tricarboxymethyl propane oleate purified material |
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| CN108295821A true CN108295821A (en) | 2018-07-20 |
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| CN201711262956.9A Withdrawn CN108295821A (en) | 2017-12-04 | 2017-12-04 | A kind of preparation method of tricarboxymethyl propane oleate purified material |
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Application publication date: 20180720 |