CN108097220A - A kind of preparation method of diethyl sebacate sorbing material - Google Patents
A kind of preparation method of diethyl sebacate sorbing material Download PDFInfo
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- CN108097220A CN108097220A CN201711151693.4A CN201711151693A CN108097220A CN 108097220 A CN108097220 A CN 108097220A CN 201711151693 A CN201711151693 A CN 201711151693A CN 108097220 A CN108097220 A CN 108097220A
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- Prior art keywords
- diethyl sebacate
- sorbing material
- vinylidene
- preparation
- material according
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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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- 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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of preparation methods of diethyl sebacate sorbing material.By weight, vinylidene, diallyl p phthalate are added in a kettle, allyl disulfide, southern 3 allyl carboxylates of 6 (1 ' tert-butyl dimethyl silica ethyl) 2 (2 ' ' tetrahydrofuran base) training, double (pentamethyl cyclopentene) titanium chloride, dodecyl benzene sulfonic acid, water heats up after mixing, reaction, product is filtered after reaction, washing, it is dry to get to diethyl sebacate sorbing material.
Description
Technical field
The present invention relates to a kind of preparation method of sorbing material, especially a kind of system of diethyl sebacate sorbing material
Preparation Method.
Background technology
Diethyl sebacate, English name：Diethyl sebacate, it is colourless to light yellow liquid, there are grape wine, fruit
And the fragrance of muskmelon, available for organic synthesis；GB 2,760 1 96 is defined as temporarily allowing the flavorant used.It is mainly used for
Prepare berries essence and the solvent as fruit type fragrance；GB 2,760 1 96 is defined as allowing the flavorant used.Mainly
For preparing the solvent of the essence such as grape, pears and fruit type essence；As plastics cold resistant plasticizer, among solvent and organic synthesis
Body.It can be additionally used in medical industry；High-molecular compound synthetic.
CN105130814A discloses a kind of method that pyrovinic acid catalysis prepares diethyl sebacate, and category catalyzes and synthesizes
The method of diethyl sebacate.It is raw material with decanedioic acid and absolute ethyl alcohol, catalyst is made with pyrovinic acid, hexamethylene makees band water
Agent, after reaction, product is neutralized, washes, distills, purifying, obtains diethyl sebacate.
CN106316850A discloses a kind of preparation method of high-purity food standard product diethyl sebacate, including with
Lower step：(1) raw material diethyl sebacate purity content is not less than 98%；(2) raw material diethyl sebacate is taken, adds in saturation chlorination
Sodium solution stirs 20-30min, places, separates water phase；(3) it is organic to be added to saturated potassium carbonate solution, 40-50 DEG C is heated to, is stirred
25-30min is mixed, is heated to 50-60 DEG C, stirs 25-30min, places, separates water phase；(4) and then after washing and drying steaming is depressurized again
It is that 99.8% (GC) is standard items to evaporate to obtain content.
Existing diethyl sebacate production or purifying technique use distillation or activated carbon adsorption mostly in purifying link,
Purification efficiency is relatively low, and technique is relatively complicated.
The content of the invention
In order to solve the above technical problems, present invention employs following technical solutions：A kind of diethyl sebacate is inhaled
The preparation method of enclosure material, comprises the following steps：
By weight, vinylidene, diallyl p phthalate, allyl disulfide, 6- are added in a kettle
(1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates, double (pentamethyl rings penta
Alkene) titanium chloride, dodecyl benzene sulfonic acid, water is warming up to 80-90 DEG C, reacts 5-15h, produce after reaction after mixing
Object is filtered, washing, dry to get to diethyl sebacate sorbing material.
The diallyl p phthalate, quality dosage are the 1-3% of vinylidene.
The allyl disulfide, quality dosage are the 0.5-1.5% of vinylidene.
Described 6- (1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- carboxylic acid allyls
Ester, quality dosage are the 0.01-0.1% of vinylidene.
Described double (pentamethyl cyclopentene) titanium chloride, quality dosage are the 0.1-0.3% of vinylidene.
The dodecyl benzene sulfonic acid, quality dosage are the 0.5-1.5% of vinylidene.
The water, quality dosage are the 400-800% of vinylidene.
The vinylidene, diallyl p phthalate, allyl disulfide, 6- (1 '-fert-butyidimethylsilyls
Silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates, double (pentamethyl cyclopentene) titanium chloride, dodecane
Base benzene sulfonic acid is commercial product.
Beneficial effects of the present invention：
（1）Adsorbent product has stronger solvent resistance, shock resistance and heat resistance, non-breakable, is easily isolated.
（2）Adsorbent product adsorption rate is fast, there is certain specific aim for the impurity in diethyl sebacate product.
Specific embodiment
Embodiment 1
In a kettle, vinylidene 100Kg, diallyl p phthalate 2Kg, allyl disulfide 1Kg, 6- are added in
(1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates 0.05Kg, double (pentamethyls
Cyclopentene) titanium chloride 0.2Kg, dodecyl benzene sulfonic acid 1Kg, water 600Kg is warming up to 85 DEG C, reacts 10h after mixing,
Product is filtered after reaction, washing, dry to get to diethyl sebacate sorbing material.
Embodiment 2
In a kettle, vinylidene 100Kg, diallyl p phthalate 1Kg, allyl disulfide 0.5Kg are added in,
6- (1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates 0.01Kg, double (five first
Cyclopentene) titanium chloride 0.1Kg, dodecyl benzene sulfonic acid 0.5Kg, water 400Kg is warming up to 80 DEG C after mixing, reaction
5h, product is filtered after reaction, washing, dry to get to diethyl sebacate sorbing material.
Embodiment 3
In a kettle, vinylidene 100Kg, diallyl p phthalate 3Kg, allyl disulfide 1.5Kg are added in,
6- (1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates 0.1Kg, double (five first
Cyclopentene) titanium chloride 0.3Kg, dodecyl benzene sulfonic acid 1.5Kg, water 800Kg is warming up to 90 DEG C after mixing, reaction
15h, product is filtered after reaction, washing, dry to get to diethyl sebacate sorbing material.
Comparative example 1
6- (1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates are added without,
His condition is the same as embodiment 1.
Comparative example 2
Double (pentamethyl cyclopentene) titanium chloride are added without, other conditions are the same as embodiment 1.
Embodiment 4
Sample of sorbent obtained by embodiment 1-3 and comparative example 1-4 is added in diethyl sebacate crude product, decanedioic acid diethyl
Ester mass percentage content is 78%, is stirred evenly, and is filtered, and the diethyl sebacate product after adsorption and purification is obtained after dry, is surveyed
Its fixed diethyl sebacate purity.It is shown in Table 1：
Table 1：Diethyl sebacate product purity ratio after the diethyl sebacate adsorbent adsorption treatment that different process is produced
Compared with.
Claims (7)
1. a kind of preparation method of diethyl sebacate sorbing material, it is characterised in that include the following steps：
By weight, vinylidene, diallyl p phthalate, allyl disulfide, 6- are added in a kettle
(1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates, double (pentamethyl rings penta
Alkene) titanium chloride, dodecyl benzene sulfonic acid, water is warming up to 80-90 DEG C, reacts 5-15h, produce after reaction after mixing
Object is filtered, washing, dry to get to diethyl sebacate sorbing material.
2. a kind of preparation method of diethyl sebacate sorbing material according to claim 1, it is characterised in that：It is described
Diallyl p phthalate, quality dosage be vinylidene 1-3%.
3. a kind of preparation method of diethyl sebacate sorbing material according to claim 1, it is characterised in that：It is described
Allyl disulfide, quality dosage be vinylidene 0.5-1.5%.
4. a kind of preparation method of diethyl sebacate sorbing material according to claim 1, it is characterised in that：It is described
6- (1 '-tert-butyl dimethyl silica ethyl) -2- (2 ' '-tetrahydrofuran base) Pei Nan -3- allyl carboxylates, quality dosage
For the 0.01-0.1% of vinylidene.
5. a kind of preparation method of diethyl sebacate sorbing material according to claim 1, it is characterised in that：It is described
Double (pentamethyl cyclopentene) titanium chloride, quality dosage is the 0.1-0.3% of vinylidene.
6. a kind of preparation method of diethyl sebacate sorbing material according to claim 1, it is characterised in that：It is described
Dodecyl benzene sulfonic acid, quality dosage be vinylidene 0.5-1.5%.
7. a kind of preparation method of diethyl sebacate sorbing material according to claim 1, it is characterised in that：It is described
Water, quality dosage be vinylidene 400-800%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711151693.4A CN108097220A (en) | 2017-11-19 | 2017-11-19 | A kind of preparation method of diethyl sebacate sorbing material |
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| CN201711151693.4A CN108097220A (en) | 2017-11-19 | 2017-11-19 | A kind of preparation method of diethyl sebacate sorbing material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582844A (en) * | 2021-08-12 | 2021-11-02 | 山东元利科技有限公司 | Method for removing monoester compound from sebacate compound |
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2017
- 2017-11-19 CN CN201711151693.4A patent/CN108097220A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582844A (en) * | 2021-08-12 | 2021-11-02 | 山东元利科技有限公司 | Method for removing monoester compound from sebacate compound |
| CN113582844B (en) * | 2021-08-12 | 2023-05-26 | 山东元利科技有限公司 | Method for removing monoester compound from sebacate compound |
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Application publication date: 20180601 |