CN111185230A - Method for separating and recovering catalyst in reaction liquid of urea and polyalcohol - Google Patents
Method for separating and recovering catalyst in reaction liquid of urea and polyalcohol Download PDFInfo
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- CN111185230A CN111185230A CN202010068346.0A CN202010068346A CN111185230A CN 111185230 A CN111185230 A CN 111185230A CN 202010068346 A CN202010068346 A CN 202010068346A CN 111185230 A CN111185230 A CN 111185230A
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Abstract
The invention discloses a method for separating and recovering a catalyst in a reaction liquid of urea and polyalcohol. The reaction solution of urea and polyhydric alcohol containing catalyst enters an evaporator, after reaction, the catalyst, biuret, a small amount of cyclic carbonate, polyhydric alcohol and intermediate product obtained from the lower part of the evaporator are transferred to a dryer, and the catalyst mixture is dried; mixing the gas phase products at the upper part of the mixed gas evaporator obtained at the upper part of the dryer, and then separating; and (2) feeding the catalyst, biuret and other organic matters without boiling points obtained from the lower part of the dryer into a high-temperature roasting device, carrying out high-temperature roasting treatment on the catalyst mixture, obtaining a gas-phase product of the decomposition of the organic matters without boiling points from the upper part, then feeding the gas-phase product into a Selective Catalytic Reduction (SCR) device for further denitration treatment, and continuously applying the fresh catalyst obtained from the lower part to the catalytic reaction process of urea and polyhydric alcohol. The invention realizes the high-efficiency separation and the repeated use of the catalyst.
Description
Technical Field
The invention relates to a method for separating and recovering a catalyst in a reaction liquid of urea and polyalcohol, in particular to a method for separating a catalyst for preparing cyclic carbonate from urea and polyalcohol, which is suitable for a reaction process for producing the cyclic carbonate, alkali metal oxide or alkali metal salt as the catalyst by the reaction of the urea and the polyalcohol. Belongs to the field of fine chemical engineering.
Background
Cyclic carbonate (ethylene carbonate, propylene carbonate, glycerol carbonate, etc.) is a new type of "green" organic compound which has wide application and is very well valued at home and abroad. In particular, the method can be applied to the fields of extraction separation of mixtures, organic synthesis (synthetic polycarbonate resin, phenolic resin and degradable medical high polymer materials), high-energy density battery electrolyte, cosmetic additives, supercritical fluid separation technology and the like.
In the reaction process of preparing the cyclic carbonate from the urea and the polyhydric alcohol, the catalyst is dissolved or remained in the organic solvent, so that the product purity of the cyclic carbonate is reduced, and the continuous operation of the subsequent working procedure is influenced. Therefore, the separation and recovery of the catalyst in the reaction liquid have important research value for the practical industrial production process.
At present, in the process of preparing propylene carbonate by reacting urea with 1, 2-propylene glycol, an alkali metal oxide or alkali metal salt catalyst is recovered, after a large-particle catalyst is separated by filtration, the catalyst dissolved in an organic solvent is separated by a film evaporator for the second time (see Chinese patent CN 204310990U), but because substances such as biuret exist in the process (the content of the biuret carried in raw material urea is about 0.8 wt%), the solution viscosity after the reaction is extremely high, and the problems that the catalyst is difficult to filter, cannot be continuously operated and the like occur.
Disclosure of Invention
The invention aims to provide a method for continuously separating and recovering a catalyst in a reaction liquid of urea and polyalcohol.
The invention relates to a method for separating and recovering a catalyst in a reaction liquid for preparing cyclic carbonate from urea and polyhydric alcohol, which mainly comprises the following steps: the method comprises the following steps of evaporating, drying and roasting at high temperature. The whole process equipment has the advantages of low investment, high catalyst recovery efficiency and the like, and meets the technical requirements of high efficiency and energy conservation of industrial practical production.
The invention provides a method for separating and recovering a catalyst in a reaction liquid of urea and polyalcohol, which comprises the following steps:
(1) feeding a reaction solution (L1) of urea and polyhydric alcohol containing a catalyst into an evaporator (E1), and obtaining an evaporator upper gas-phase product G1, namely polyhydric alcohol, cyclic carbonate, an intermediate product (hydroxyethyl carbamate, hydroxypropyl carbamate, 1, 2-dihydroxypropyl carbamate) and the like, from the upper gas phase of the evaporator under the conditions that the pressure is 30-210 mmHg, the temperature is 130-200 ℃ and the time is 3-12 hours; the lower part of the evaporator is provided with a catalyst (L2) containing a small amount of biuret, a small amount of cyclic carbonate, a small amount of polyhydric alcohol and an intermediate product;
(2) transferring the catalyst, biuret and a small amount of cyclic carbonate, polyol, intermediate product and the like (L2) obtained at the lower part of the evaporator in the step (1) to a dryer (D1), and drying the catalyst mixture under the conditions of normal pressure, 150-350 ℃ and 4-12 h; the mixed gas (G2) -cyclic carbonate, polyhydric alcohol and intermediate product obtained from the upper part of the dryer are mixed with the gas-phase product G1 from the upper part of the evaporator in the step (1) and then separated.
(3) And (3) feeding the catalyst, biuret and other non-boiling point organic matters (S1) obtained at the lower part of the dryer in the step (2) into a high-temperature roasting device (F1), roasting the catalyst mixture at high temperature under the conditions of normal pressure, 200-1000 ℃ and 1-12 h, obtaining gas-phase products of the decomposition of the non-boiling point organic matters such as biuret and triurea at the upper part, then connecting the gas-phase products into a Selective Catalytic Reduction (SCR) device for further denitration treatment, and continuously applying the fresh catalyst obtained at the lower part to the catalytic reaction process of urea and polyhydric alcohol, thereby realizing the efficient separation and the repeated use of the catalyst.
The above scheme is further illustrated as follows:
the catalyst is one or a mixture of more of sodium carbonate, potassium carbonate, magnesium carbonate, zinc carbonate, lithium carbonate, zirconium oxide, barium oxide, gallium oxide, magnesium oxide, calcium oxide, zinc oxide, strontium oxide, aluminum oxide, ferric oxide, ferroferric oxide, zinc acetate, magnesium acetate, calcium acetate and iron acetate.
The polyhydric alcohol is one of ethylene glycol, propylene glycol and glycerol, and correspondingly, the cyclic organic carbonate is one of ethylene carbonate, propylene carbonate and glycerol carbonate.
The evaporator is one of a scraper evaporator or a falling film evaporator.
The dryer is one of a double-cone rotary dryer or a box type dryer.
The high-temperature roaster is one of a mesh belt kiln, a tunnel kiln, a roller kiln, a rotary roasting furnace or a shuttle kiln.
The invention has the beneficial effects that: the mixed liquid directly enters the evaporator without being filtered, so that the blockage of viscous substances such as biuret and the like to a filtering system is avoided, and then the catalyst is thoroughly separated by drying and adopting high-temperature roasting, so that the continuous operation of a reaction system is realized, the catalyst loss is reduced, the catalyst recovery efficiency is improved, and the production cost is reduced.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
In the figure: l1: a reaction solution of urea and polyhydric alcohol containing a catalyst; e1: an evaporator; g1: vapor phase product in the upper part of the evaporator; l2: a catalyst comprising a small amount of biuret, a small amount of cyclic carbonate, a small amount of polyol, and intermediates; d1: a dryer; g2: cyclic carbonate, polyol, intermediate; s1: catalysts, biuret and other non-boiling point organics; f1: a high temperature roasting device; s is a catalyst; h: an SCR system.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
The invention provides a method for separating and recovering a catalyst in a reaction liquid of urea and polyalcohol, which comprises the following steps:
(1) the reaction liquid L1 of urea and polyhydric alcohol containing catalyst enters an evaporator E1, and after reaction, the gas phase at the upper part of the evaporator obtains a gas phase product G1 at the upper part of the evaporator, which is polyhydric alcohol, cyclic carbonate and an intermediate product; the catalyst L2 containing a small amount of biuret, a small amount of cyclic carbonate, a small amount of polyol and an intermediate product is obtained at the lower part of the evaporator;
(2) transferring the catalyst, biuret, a small amount of cyclic carbonate, polyol and intermediate product obtained from the lower part of the evaporator in the step (1) to a dryer D1, and drying the catalyst mixture; the mixed gas G2 obtained at the upper part of the dryer is cyclic carbonate, polyhydric alcohol and an intermediate product, is mixed with the gas-phase product G1 at the upper part of the evaporator in the step (1), and is separated;
(3) and (3) feeding the catalyst, biuret and other organic matters without boiling point S1 obtained from the lower part of the dryer in the step (2) into a high-temperature roasting device F1, carrying out high-temperature roasting treatment on the catalyst mixture, obtaining a gas-phase product of decomposition of the organic matters without boiling point from the upper part, then switching into a selective catalytic reduction SCR device for further denitration treatment, and continuously applying the fresh catalyst obtained from the lower part to the catalytic reaction process of urea and polyhydric alcohol, thereby realizing efficient separation and reuse of the catalyst.
In the above separation and recovery method, the catalyst is one or a mixture of more of sodium carbonate, potassium carbonate, magnesium carbonate, zinc carbonate, lithium carbonate, zirconium oxide, barium oxide, gallium oxide, magnesium oxide, calcium oxide, zinc oxide, strontium oxide, aluminum oxide, ferric oxide, ferroferric oxide, zinc acetate, magnesium acetate, calcium acetate, and iron acetate.
In the above separation and recovery method, the polyhydric alcohol is one of ethylene glycol, propylene glycol and glycerol, and correspondingly, the cyclic carbonate is one of ethylene carbonate, propylene carbonate and glycerol carbonate.
In the above separation and recovery method, the reaction conditions in the evaporator are as follows: the pressure is 30-210 mmHg, the temperature is 130-200 ℃, and the reaction time is 3-12 h.
In the above separation and recovery method, the intermediate product comprises hydroxyethyl carbamate, hydroxypropyl carbamate or 1, 2-dihydroxypropyl carbamate.
In the above separation and recovery method, the evaporator is one of a scraper evaporator and a falling film evaporator.
In the above separation and recovery method, the reaction conditions in the dryer are as follows: the reaction is carried out at the normal pressure, the temperature of 150-350 ℃ and the reaction time of 4-12 h.
In the above separation and recovery method, the dryer is one of a double-cone rotary dryer or a box dryer
In the above separation and recovery method, the reaction conditions in the high-temperature roasting device are as follows: the reaction is carried out at normal pressure and temperature of 200-1000 ℃ for 1-12 h.
In the separation and recovery method, the high-temperature roasting device is one of a mesh belt kiln, a tunnel roasting kiln, a vertical roasting furnace, a roller kiln, a rotary roasting furnace or a shuttle kiln.
Example 1:
this example is used for the separation of catalyst in the preparation of ethylene carbonate from urea and ethylene glycol (the catalyst is a zinc oxide and calcium oxide complex with a molar ratio of 1: 1). First, the mixed liquid enters a scraper evaporator E1, and under the conditions of 150 mmHg, 145 ℃ and 6 h, the vapor phase product G1: ethylene carbonate, hydroxyethyl carbamate, ethylene glycol, and the like are evaporated from the upper part of the evaporator and then separated, and the organic matter such as the catalyst and the non-boiling biuret at the lower part of the evaporator is introduced into a double-cone rotary dryer D1. Secondly, under the conditions of normal pressure, 250 ℃ and 8 hours, a small amount of light components (propylene glycol, propylene carbonate and the like) obtained at the upper part of the dryer and a gas-phase product obtained at the upper part of the evaporator are mixed and then separated, and a catalyst obtained at the lower part of the dryer and a non-boiling point mixture such as biuret enter a high-temperature roasting device F1-mesh belt kiln. And finally, roasting at the normal pressure, 850 ℃ and 4 h, obtaining gas-phase products of decomposing non-boiling point organic matters such as biuret and triurea at the upper part, then accessing a Selective Catalytic Reduction (SCR) device for cleaning treatment, continuously applying the fresh catalyst obtained at the lower part to the catalytic reaction process of urea and ethylene glycol, and ensuring that the catalyst recovery rate is 100%.
Example 2:
this example is used for the separation of catalyst in the preparation of propylene carbonate from urea and propylene glycol (the catalyst is a compound of zinc oxide and calcium oxide, the molar ratio is 1: 1). Firstly, the mixed liquid enters a falling-film evaporator E1, and under the conditions of the pressure of 210mmHg, 140 ℃ and 8 hours, the upper gas-phase product G1: products such as propylene carbonate, hydroxypropyl carbamate, propylene glycol and the like are evaporated from the upper part of the evaporator and then separated, and the catalyst and organic matters such as non-boiling biuret and the like at the lower part of the evaporator enter a chamber dryer D1. Then, under the conditions of normal pressure, 250 ℃ and 10 hours, a small amount of light components (ethylene glycol, ethylene carbonate and the like) obtained at the upper part of the dryer and a gas-phase product obtained at the upper part of the evaporator are mixed and then separated, and a catalyst obtained at the lower part of the dryer and a non-boiling point mixture such as biuret enter a high-temperature roasting device F1, namely a tunnel kiln. And finally, roasting at the normal pressure, 850 ℃ and 6 h, obtaining gas-phase products of decomposing non-boiling point organic matters such as biuret and triurea at the upper part, then accessing a Selective Catalytic Reduction (SCR) device for cleaning treatment, continuously applying the fresh catalyst obtained at the lower part to the catalytic reaction process of urea and propylene glycol, and ensuring that the catalyst recovery rate is 100%.
Example 3:
this example is used for the separation of catalyst in the preparation of glycerol carbonate from urea and glycerol (the catalyst is a zinc oxide and calcium oxide complex with a molar ratio of 1: 1). First, the mixture was introduced into a wiped film evaporator E1, and the vapor phase product G1: products such as glycerin carbonate, 1, 2-dihydroxypropyl amino carbonate, and glycerin were distilled out from the upper part of the evaporator and then separated, and the organic substances such as the catalyst and the non-boiling biuret at the lower part of the evaporator were introduced into a dryer D1. Then, under the conditions of normal pressure, 350 ℃ and 12 hours, a small amount of light components (glycerin, glycerin carbonate, etc.) obtained at the upper part of the dryer and the gas-phase product obtained at the upper part of the evaporator were mixed and then separated, and the catalyst obtained at the lower part of the dryer and a non-boiling point mixture such as biuret were introduced into a high-temperature calcination apparatus F1. And finally, roasting at normal pressure, 1000 ℃ and 12 h, obtaining gas-phase products of non-boiling point organic matter decomposition such as biuret and triurea at the upper part, then accessing a Selective Catalytic Reduction (SCR) device for cleaning treatment, and continuously applying the fresh catalyst obtained at the lower part to the catalytic reaction process of urea and glycerol, wherein the recovery rate of the catalyst is 100%.
Example 4:
this example is used for the separation of catalyst in the process of preparing propylene carbonate from urea and propylene glycol (the catalyst is a compound of zinc carbonate and magnesium carbonate with a molar ratio of 1: 1). First, the mixture was introduced into an evaporator E1, and the vapor phase product G1: the products such as propylene carbonate, hydroxypropyl carbamate, propylene glycol and the like were distilled out from the upper part of the evaporator and then separated, and the organic substances such as the catalyst and the non-boiling biuret at the lower part of the evaporator were introduced into a dryer D1. Then, under the conditions of normal pressure, 150 ℃ and 4 hours, a small amount of light components (ethylene glycol, ethylene carbonate and the like) obtained at the upper part of the dryer and the gas-phase product obtained at the upper part of the evaporator were mixed and then separated, and the catalyst obtained at the lower part of the dryer and a non-boiling point mixture such as biuret were introduced into a high-temperature calcination apparatus F1. And finally, roasting at normal pressure, 200 ℃ and 6 h, obtaining gas-phase products of non-boiling point organic matters such as biuret and triurea decomposed at the upper part, then accessing a Selective Catalytic Reduction (SCR) device for cleaning treatment, and continuously applying the fresh catalyst obtained at the lower part to the catalytic reaction process of urea and propylene glycol, wherein the recovery rate of the catalyst is 100%.
Example 5:
this example is used for the separation of catalyst in the preparation of propylene carbonate from urea and propylene glycol (the catalyst is a compound of zinc acetate and magnesium acetate, and the molar ratio is 1: 1). First, the mixture was introduced into an evaporator E1, and the vapor phase product G1: the products such as propylene carbonate, hydroxypropyl carbamate, propylene glycol and the like were distilled out from the upper part of the evaporator and then separated, and the organic substances such as the catalyst and the non-boiling biuret at the lower part of the evaporator were introduced into a dryer D1. Then, under the conditions of normal pressure, 150 ℃ and 4 hours, a small amount of light components (ethylene glycol, ethylene carbonate and the like) obtained at the upper part of the dryer and the gas-phase product obtained at the upper part of the evaporator were mixed and then separated, and the catalyst obtained at the lower part of the dryer and a non-boiling point mixture such as biuret were introduced into a high-temperature calcination apparatus F1. And finally, roasting at normal pressure, 200 ℃ and 6 h, obtaining gas-phase products of non-boiling point organic matters such as biuret and triurea decomposed at the upper part, then accessing a Selective Catalytic Reduction (SCR) device for cleaning treatment, and continuously applying the fresh catalyst obtained at the lower part to the catalytic reaction process of urea and propylene glycol, wherein the recovery rate of the catalyst is 100%.
Claims (10)
1. A method for separating and recovering a catalyst in a reaction liquid of urea and polyhydric alcohol is characterized by comprising the following steps:
(1) the reaction liquid (L1) of urea containing catalyst and polyhydric alcohol enters an evaporator (E1), after the reaction, the gas phase at the upper part of the evaporator obtains a gas phase product (G1) at the upper part of the evaporator, and the gas phase product is polyhydric alcohol, cyclic carbonate and an intermediate product; the lower part of the evaporator is provided with a catalyst (L2) containing a small amount of biuret, a small amount of cyclic carbonate, a small amount of polyhydric alcohol and an intermediate product;
(2) transferring the catalyst, biuret, a small amount of cyclic carbonate, polyol and intermediate product obtained from the lower part of the evaporator in the step (1) to a dryer (D1), and drying the catalyst mixture; the mixed gas (G2) obtained at the upper part of the dryer is cyclic carbonate, polyhydric alcohol and an intermediate product, is mixed with the gas-phase product (G1) at the upper part of the evaporator in the step (1), and is separated;
(3) and (3) feeding the catalyst, biuret and other organic matters without boiling points (S1) obtained from the lower part of the dryer in the step (2) into a high-temperature roasting device (F1), roasting the catalyst mixture at high temperature, obtaining a gas-phase product of decomposition of the organic matters without boiling points from the upper part, then switching into a selective catalytic reduction device for further denitration treatment, and continuously applying the fresh catalyst obtained from the lower part to the catalytic reaction process of urea and polyhydric alcohol, thereby realizing efficient separation and reuse of the catalyst.
2. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the catalyst is one or a mixture of more of sodium carbonate, potassium carbonate, magnesium carbonate, zinc carbonate, lithium carbonate, zirconium oxide, barium oxide, gallium oxide, magnesium oxide, calcium oxide, zinc oxide, strontium oxide, aluminum oxide, ferric oxide, ferroferric oxide, zinc acetate, magnesium acetate, calcium acetate and iron acetate.
3. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the polyhydric alcohol is one of ethylene glycol, propylene glycol and glycerol, and correspondingly, the cyclic carbonate is one of ethylene carbonate, propylene carbonate and glycerol carbonate.
4. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the reaction conditions in the evaporator were: the pressure is 30-210 mmHg, the temperature is 130-200 ℃, and the reaction time is 3-12 h.
5. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the intermediate product comprises hydroxyethyl carbamate, hydroxypropyl carbamate or 1, 2-dihydroxypropyl carbamate.
6. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the evaporator is one of a scraper evaporator or a falling film evaporator.
7. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the reaction conditions in the dryer were: the reaction is carried out at the normal pressure, the temperature of 150-350 ℃ and the reaction time of 4-12 h.
8. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the dryer is one of a double-cone rotary dryer or a box type dryer.
9. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the reaction conditions in the high-temperature roasting device are as follows: the reaction is carried out at normal pressure and temperature of 200-1000 ℃ for 1-12 h.
10. The method according to claim 1, wherein the catalyst in the reaction solution of urea and polyol is separated and recovered by: the high-temperature roasting device is one of a mesh belt kiln, a tunnel roasting kiln, a vertical roasting furnace, a roller kiln, a rotary roasting furnace or a shuttle kiln.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111841574A (en) * | 2020-08-28 | 2020-10-30 | 华东理工大学 | Catalyst regeneration method for preparing propylene (or ethylene) carbonate by urea alcoholysis method |
| CN116237061A (en) * | 2022-12-19 | 2023-06-09 | 中国科学院福建物质结构研究所 | Method for recovering catalyst of co-production reaction of oxamide and methyl carbamate |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450317A (en) * | 2007-12-03 | 2009-06-10 | 中国科学院成都有机化学有限公司 | Carbonic allyl ester preparation catalyst through catalyzing urea and 1,2-propylene glycol |
| CN102304050A (en) * | 2011-07-25 | 2012-01-04 | 屈强好 | Method for continuously rectifying dimethyl carbonate and 1,2-propylene glycol |
| EP2873661A1 (en) * | 2013-11-14 | 2015-05-20 | Arkema France | Synthesis process of trimethylene carbonate from 1,3-propanediol and urea by heterogeneous catalysis |
| WO2016082766A1 (en) * | 2014-11-28 | 2016-06-02 | 中国科学院大连化学物理研究所 | Separating method for polyol mixtures with close boiling points |
| CN107353207A (en) * | 2017-08-21 | 2017-11-17 | 中石化上海工程有限公司 | A kind of method and its system of urea two-step method production dimethyl carbonate |
| CN110156742A (en) * | 2019-07-02 | 2019-08-23 | 中国科学院过程工程研究所 | A kind of method of ionic liquid-catalyzed urea and dihydric alcohol synthesizing annular carbonate |
| CN110256397A (en) * | 2019-07-24 | 2019-09-20 | 河南大学 | The extracting method of biuret during urea and polyol reaction cyclic carbonate |
| CN110339867A (en) * | 2019-07-24 | 2019-10-18 | 河南大学 | Urea and polyol reaction prepare cyclic carbonate catalyst recovery method |
-
2020
- 2020-01-21 CN CN202010068346.0A patent/CN111185230A/en not_active Withdrawn
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450317A (en) * | 2007-12-03 | 2009-06-10 | 中国科学院成都有机化学有限公司 | Carbonic allyl ester preparation catalyst through catalyzing urea and 1,2-propylene glycol |
| CN102304050A (en) * | 2011-07-25 | 2012-01-04 | 屈强好 | Method for continuously rectifying dimethyl carbonate and 1,2-propylene glycol |
| EP2873661A1 (en) * | 2013-11-14 | 2015-05-20 | Arkema France | Synthesis process of trimethylene carbonate from 1,3-propanediol and urea by heterogeneous catalysis |
| WO2016082766A1 (en) * | 2014-11-28 | 2016-06-02 | 中国科学院大连化学物理研究所 | Separating method for polyol mixtures with close boiling points |
| CN107353207A (en) * | 2017-08-21 | 2017-11-17 | 中石化上海工程有限公司 | A kind of method and its system of urea two-step method production dimethyl carbonate |
| CN110156742A (en) * | 2019-07-02 | 2019-08-23 | 中国科学院过程工程研究所 | A kind of method of ionic liquid-catalyzed urea and dihydric alcohol synthesizing annular carbonate |
| CN110256397A (en) * | 2019-07-24 | 2019-09-20 | 河南大学 | The extracting method of biuret during urea and polyol reaction cyclic carbonate |
| CN110339867A (en) * | 2019-07-24 | 2019-10-18 | 河南大学 | Urea and polyol reaction prepare cyclic carbonate catalyst recovery method |
Non-Patent Citations (2)
| Title |
|---|
| 刘猛帅: "CO2转化合成环状碳酸酯多功能催化剂的设计及催化机制", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
| 王元 等: "尿素与丙二醇合成碳酸丙烯酯的中试研究", 《化肥工业》 * |
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| CN111841574A (en) * | 2020-08-28 | 2020-10-30 | 华东理工大学 | Catalyst regeneration method for preparing propylene (or ethylene) carbonate by urea alcoholysis method |
| CN116237061A (en) * | 2022-12-19 | 2023-06-09 | 中国科学院福建物质结构研究所 | Method for recovering catalyst of co-production reaction of oxamide and methyl carbamate |
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