CN108079958A - A kind of preparation method of 2- imidazolidinones sorbing material - Google Patents
A kind of preparation method of 2- imidazolidinones sorbing material Download PDFInfo
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- CN108079958A CN108079958A CN201711149142.4A CN201711149142A CN108079958A CN 108079958 A CN108079958 A CN 108079958A CN 201711149142 A CN201711149142 A CN 201711149142A CN 108079958 A CN108079958 A CN 108079958A
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- imidazolidinones
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/28—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D233/30—Oxygen or sulfur atoms
- C07D233/32—One oxygen atom
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Abstract
The present invention relates to a kind of preparation methods of 2 imidazolidinone sorbing material.By weight, hollow glass micro-ball, diallyl diethoxy silane are added in a kettle, 2,3 dicarboxylic acid esters of diallyl naphthalene, 4,51,3 dioxole of dimethyl, 2 ketone, acrylic acid 1,1,1,3,3,3 hexafluoro isopropyl esters, 4 (5 methane acyl furans, 2 base) benzene sulfonic acids, 1 pi-allyl, 3 ethyl imidazol(e) tetrafluoroborate ionic liquid, ammonium persulfate, water, neopelex, it heats up after stirring evenly, reaction, after product it is filtered, washing, it is dry to get to 2 imidazolidinone sorbing materials.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of preparation side of 2- imidazolidinones sorbing material
Method.
Background technology
2- imidazolidinones remove aldehyde field, such as available for all kinds of：High-performance formaldehyde scavenger, the potent work of home air formaldehyde
Power enzyme, formaldehyde are long-acting to melt matchmaker, glue aldehyde remover, photocatalyst, floor taste removal nursing wax, furniture eliminating smell agent, automobile-used eliminating smell agent, spinning
Auxiliary agent is knitted except aldehyde intermediate, resin are except aldehyde etc.；In addition, can be additionally used in fabric crease-shedding finishing agent in textile industry, tear-proof is whole
Manage agent；In medical industry, it can be used as various new antibiotic intermediates, such as mezlocillin, azlocillin, can also be used as anti-
The intermediate of Schistosomicide, and can be as the basic material of third generation penicillin；In biological field, it can produce plant growth
Conditioning agent, fungicide, inhibitor, herbicide etc., such as：N-- chloroformyl -2- imidazolidinones, 1- chloroformyl -3- acetyl group -
2- imidazolidinones, 1-chlorocarbonyl-3-methylsulphonyl-2-imidazolidone, N- ethoxy -2- imidazolidinones, 1- mesyls -2-
Imidazolidinone, 1,3- dimethyl -2- imidazolidinones, 1- acetyl group -2- imidazolidinones etc.；Fabric crease-shedding finishing agent and aldehyde removing agent,
Make crosslinking agent in rubber, resin, PA6 etc.；Make piptonychia aldehyde agent in poly- EVA, all kinds of water based paints, adhesive, pigment, paint etc.；
Being individually added into coating, which possesses coating, absorbs decomposing formaldehyde function；Wetting, anti-blocking and scattered work are played in ink-jet printing ink
With；Chelating agent and formaldehyde absorbent in photosensitive material；It is used as in paper industry except formaldehyde treated agent.It is and all kinds of with fresh air
Agent, the main component of aldehyde remover, the important intermediate of artificial synthesized penicillin.
CN103497157B discloses a kind of synthetic method of 2- imidazolidinones, is related to 2- imidazolidinones.Technique letter is provided
A kind of synthetic method of single, at low cost 2- imidazolidinones.1）By catalyst sulfamic acid, solvent methanol, ethylenediamine, carbonic acid two
Methyl esters is added sequentially to react in heating response device, and the temperature of the reaction is 20~80 DEG C, and the time of reaction is 1~5h；
2）It is continuously heating to 120~180 DEG C, reaction 10~generate afterwards for 24 hours target product 2- imidazolidinones；3）It crosses and filters out after reaction
Catalyst sulfamic acid is removed, removing solvent methanol is up to crude product 2- imidazolidinones；4）By step 3）Obtained crude product 2- miaows
Oxazolidone purifies, and obtains product 2- imidazolidinones.
CN102030711B discloses a kind of synthetic method of 2- imidazolidinones, what this method was realized in the following way：
The mixture at least heated by two kinds of components of ethylenediamine and urea is evaporated and collects to have obtained target product.
Existing synthesis or the technique of purification 2- imidazolidinones, are purified mostly using the method for recrystallization or distillation,
Energy consumption is high, and time-consuming；Therefore, research and development are a kind of high for 2- imidazolidinone products adsorption efficiency, the fast 2- imidazolidines of adsorption rate
Ketone purification is necessary with adsorbent.
The content of the invention
The purpose of the present invention is：There is provided a kind of preparation method of 2- imidazolidinones sorbing material, it is characterised in that prepare
Step includes：
By weight, hollow glass micro-ball is added in a kettle, diallyl diethoxy silane, diallyl naphthalene -2,
3- dicarboxylic acid esters, 4,5- dimethyl -1,3- dioxole -2- ketone, 1,1,1,3,3,3- hexafluoro isopropyl ester of acrylic acid, 4-
(5- methane acyl furans -2- bases) benzene sulfonic acid, 1- pi-allyl -3- ethyl imidazol(e) tetrafluoroborate ionic liquids, ammonium persulfate, water, ten
Dialkyl benzene sulfonic acids sodium, is warming up to 90-110 DEG C after stirring evenly, react 6-14h, after product it is filtered, wash, it is dry,
Obtain 2- imidazolidinone sorbing materials.
The diallyl diethoxy silane, quality dosage are the 1-3% of hollow glass micro-ball.The diene
Propyl naphthalene -2,3- dicarboxylic acid esters, quality dosage are the 0.5-1.5% of hollow glass micro-ball.4,5- dimethyl-the 1,3-
Dioxole -2- ketone, quality dosage are the 0.5-1.5% of hollow glass micro-ball.The acrylic acid 1,1,1,3,3,
3- hexafluoro isopropyl esters, quality dosage are the 0.1-0.5% of hollow glass micro-ball.Described 4- (the 5- methane acyl furans -2- bases) benzene
Sulfonic acid, quality dosage are the 0.1-0.5% of hollow glass micro-ball.
1- pi-allyl -3- ethyl imidazol(e) tetrafluoroborate the ionic liquids, quality dosage are hollow glass micro-ball
0.01-0.1%.The ammonium persulfate, quality dosage are the 0.5-2% of hollow glass micro-ball.The detergent alkylate sulphur
Sour sodium, quality dosage are the 0.5-2% of hollow glass micro-ball, and the water, quality dosage is the 300- of hollow glass micro-ball
500%。
The hollow glass micro-ball, diallyl diethoxy silane, 4,5- dimethyl -1,3- Dloxoles
Alkene -2- ketone, 1,1,1,3,3,3- hexafluoro isopropyl ester of acrylic acid, 4- (5- methane acyl furans -2- bases) benzene sulfonic acid, 1- pi-allyls -3-
Ethyl imidazol(e) tetrafluoroborate ionic liquid, ammonium persulfate, water are commercial product.
The product of the present invention has the advantages that：
（1）The adsorbent product that the present invention is produced has stronger mechanical strength and endurance heat resistance, in adsorption process
It is non-breakable, not mutability, the performance adsorption effect that can stablize for a long time.
（2）The adsorbent that the present invention is produced has larger specific surface area, and compared to traditional activated carbon adsorption
Agent has certain specific aim for the organic impurity that contains in 2- imidazolidinone products, have faster adsorption rate and
The adsorption capacity of bigger.
Specific embodiment
Embodiment 1
In a kettle, hollow glass micro-ball 100Kg, diallyl diethoxy silane 2Kg, diallyl naphthalene -2,3- are added in
Dicarboxylic acid esters 1Kg, 4,5- dimethyl -1,3- dioxole -2- ketone 1Kg, 1,1,1,3,3,3- hexafluoro isopropyl of acrylic acid
Ester 0.3Kg, 4- (5- methane acyl furans -2- bases) benzene sulfonic acid 0.2Kg, 1- pi-allyl -3- ethyl imidazol(e) tetrafluoroborate ionic liquids
0.05Kg, ammonium persulfate 0.75Kg, water 400Kg, neopelex 1Kg are warming up to 100 DEG C, reaction after stirring evenly
10h, after product it is filtered, washing is dry to get to 2- imidazolidinone sorbing materials.
Embodiment 2
In a kettle, hollow glass micro-ball 100Kg, diallyl diethoxy silane 1Kg, diallyl naphthalene -2,3- are added in
Dicarboxylic acid esters 0.5Kg, 4,5- dimethyl -1,3- dioxole -2- ketone 0.5Kg, 1,1,1,3,3,3- hexafluoro of acrylic acid
Isopropyl ester 0.1Kg, 4- (5- methane acyl furans -2- bases) benzene sulfonic acid 0.1Kg, 1- pi-allyl -3- ethyl imidazol(e)s tetrafluoroborate from
Sub- liquid 0.01Kg, ammonium persulfate 0.5Kg, water 300Kg, neopelex 0.5Kg are warming up to 90 DEG C after stirring evenly,
React 6h, after product it is filtered, washing is dry to get to 2- imidazolidinone sorbing materials.
Embodiment 3
In a kettle, hollow glass micro-ball 100Kg, diallyl diethoxy silane 3Kg, diallyl naphthalene -2,3- are added in
Dicarboxylic acid esters 1.5Kg, 4,5- dimethyl -1,3- dioxole -2- ketone 1.5Kg, 1,1,1,3,3,3- hexafluoro of acrylic acid
Isopropyl ester 0.5Kg, 4- (5- methane acyl furans -2- bases) benzene sulfonic acid 0.5Kg, 1- pi-allyl -3- ethyl imidazol(e)s tetrafluoroborate from
Sub- liquid 0.1Kg, ammonium persulfate 2Kg, water 500Kg, neopelex 2Kg are warming up to 100 DEG C, reaction after stirring evenly
10h, after product it is filtered, washing is dry to get to 2- imidazolidinone sorbing materials.
Comparative example 1
4,5- dimethyl -1,3- dioxole -2- ketone is added without, other conditions are the same as embodiment 1.
Comparative example 2
1,1,1,3,3,3- hexafluoro isopropyl ester of acrylic acid is added without, other conditions are the same as embodiment 1.
Comparative example 3
4- (5- methane acyl furans -2- bases) benzene sulfonic acid is added without, other conditions are the same as embodiment 1.
Comparative example 4
1- pi-allyl -3- ethyl imidazol(e) tetrafluoroborate ionic liquids are added without, other conditions are the same as embodiment 1.
Embodiment 4
The 2- imidazolidinone crude products that mass percent concentration is about 85% are passed through equipped with 500g embodiments 1-3 and comparative example 1-4
The 1000L exchange columns of adsorbent product, 75 DEG C, flow velocity 0.5BV/h of temperature, under the conditions of adsorb purification, with gas chromatographic detection stream
Go out the mass percentage of liquid, be shown in Table 1.
Table 1：2- imidazolidinone product purities after the adsorbent product absorption that different process is produced.
Claims (9)
1. a kind of preparation method of 2- imidazolidinones sorbing material, it is characterised in that preparation process includes：
By weight, hollow glass micro-ball is added in a kettle, diallyl diethoxy silane, diallyl naphthalene -2,
3- dicarboxylic acid esters, 4,5- dimethyl -1,3- dioxole -2- ketone, 1,1,1,3,3,3- hexafluoro isopropyl ester of acrylic acid, 4-
(5- methane acyl furans -2- bases) benzene sulfonic acid, 1- pi-allyl -3- ethyl imidazol(e) tetrafluoroborate ionic liquids, ammonium persulfate, water, ten
Dialkyl benzene sulfonic acids sodium, is warming up to 90-110 DEG C after stirring evenly, react 6-14h, after product it is filtered, wash, it is dry,
Obtain 2- imidazolidinone sorbing materials.
2. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
Diallyl diethoxy silane, quality dosage are the 1-3% of hollow glass micro-ball.
3. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
Diallyl naphthalene -2,3- dicarboxylic acid esters, quality dosage are the 0.5-1.5% of hollow glass micro-ball.
4. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
4,5- dimethyl -1,3- dioxole -2- ketone, quality dosage are the 0.5-1.5% of hollow glass micro-ball.
5. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
1,1,1,3,3,3- hexafluoro isopropyl ester of acrylic acid, quality dosage are the 0.1-0.5% of hollow glass micro-ball.
6. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
4- (5- methane acyl furans -2- bases) benzene sulfonic acid, quality dosage are the 0.1-0.5% of hollow glass micro-ball.
7. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
1- pi-allyl -3- ethyl imidazol(e) tetrafluoroborate ionic liquids, quality dosage are the 0.01-0.1% of hollow glass micro-ball.
8. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
Ammonium persulfate, quality dosage are the 0.5-2% of hollow glass micro-ball, and the neopelex, quality dosage is
The 0.5-2% of hollow glass micro-ball.
9. a kind of preparation method of 2- imidazolidinones sorbing material according to claim 1, it is characterised in that：Described
Water, quality dosage are the 300-500% of hollow glass micro-ball.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5075406A (en) * | 1988-03-08 | 1991-12-24 | Mitsui Toatsu Chemicals, Inc. | Process for refining 1,3-dimethyl-2-imidazolidinone |
| CN105110406A (en) * | 2015-08-24 | 2015-12-02 | 河南师范大学 | Application of ionic liquid functional silica gel to removing phenolic pollutants in waste water |
| CN105566586A (en) * | 2016-03-04 | 2016-05-11 | 中国科学院新疆理化技术研究所 | Preparation method of benzenearsonic acid molecular imprinting polymer |
| CN106311168A (en) * | 2016-08-21 | 2017-01-11 | 王琪宇 | Preparation method for adsorbent for purifying 2-imidazolidone |
-
2017
- 2017-11-18 CN CN201711149142.4A patent/CN108079958A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5075406A (en) * | 1988-03-08 | 1991-12-24 | Mitsui Toatsu Chemicals, Inc. | Process for refining 1,3-dimethyl-2-imidazolidinone |
| CN105110406A (en) * | 2015-08-24 | 2015-12-02 | 河南师范大学 | Application of ionic liquid functional silica gel to removing phenolic pollutants in waste water |
| CN105566586A (en) * | 2016-03-04 | 2016-05-11 | 中国科学院新疆理化技术研究所 | Preparation method of benzenearsonic acid molecular imprinting polymer |
| CN106311168A (en) * | 2016-08-21 | 2017-01-11 | 王琪宇 | Preparation method for adsorbent for purifying 2-imidazolidone |
Non-Patent Citations (3)
| Title |
|---|
| 何天白，胡汉杰主编: "《功能高分子与新技术》", 31 January 2001 * |
| 刘胜新主编: "《化验员手册》", 28 February 2014 * |
| 王方主编: "《现代离子交换与吸附技术》", 30 November 2015 * |
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