CN201567298U - Production system for synthesizing oxalic ester and co-producing oxalic acid - Google Patents
Production system for synthesizing oxalic ester and co-producing oxalic acid Download PDFInfo
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- CN201567298U CN201567298U CN 200920210195 CN200920210195U CN201567298U CN 201567298 U CN201567298 U CN 201567298U CN 200920210195 CN200920210195 CN 200920210195 CN 200920210195 U CN200920210195 U CN 200920210195U CN 201567298 U CN201567298 U CN 201567298U
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- condenser
- air outlet
- oxalic acid
- barkite
- esterifier
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Abstract
The utility model relates to a production system for synthesizing oxalic ester and co-producing oxalic acid. The production system comprises a gas phase coupling carbonylation reactor, a first condenser, an oxalic ester hydrolysis reactor and an esterification reactor which are sequentially circularly connected. Since the utility model introduces the condenser and the oxalic ester hydrolysis reactor into the circulated process of CO gas phase coupling oxalic ester synthesization, various technical problems in the technique for preparing oxalic ester are solved, and oxalic ester and oxalic acid can be co-produced as well.
Description
Technical field
The utility model relates to the production system of a kind of synthesis of oxalate and coproduction oxalic acid.
Background technology
Oxalic acid, dimethyl oxalate and oxalic acid diethyl ester all are important Organic Chemicals, oxalic acid extracts in the fields such as refining, metal treatment and cleaning and polymkeric substance be synthetic in chemosynthesis, pharmacy, rare earth element and is widely used, and dimethyl oxalate and oxalic acid diethyl ester low-voltage hydrogenation can make the generally attention that important industrial chemicals ethylene glycol is subjected to chemical field especially.
Traditional oxalic acid working system is sodium formate method, ethylene glycol oxidation, carbohydrate oxidation method etc., all because of seriously polluted or backward in technique, progressively is eliminated.The traditional working system of dimethyl oxalate and oxalic acid diethyl ester is to make by oxalic acid and alcohols esterification, because the backwardness of oxalic acid traditional method is subjected to the restriction of raw material, it is comparatively backward that technological line also seems.
In 1980, Japanese UBE company (EP0046598,1981; EP0086370,1983) and U.S. union carbide corporation (EP0057630,1982) successively disclosing with CO is raw material, by means of methyl nitrite or ethyl nitrite, and be catalyzer with Pd/a-A12O3, make CO oxidation coupling connection generate the method for dimethyl oxalate or the oxalic acid diethyl ester, (CN1054765A of Fujian Inst. of Matter Structure, Chinese Academy of Sciences simultaneously, 1991), University Of Tianjin (CN1149047,1997) and Shanghai Communications University (CN101190884) also disclose similar method.The reaction principle of this method is as follows:
Total reaction is: 2CO+2CH
3OH+1/2O
2→ (COOCH
3)
2+ H
2O (1)
Coupling connection carbonylation:
Esterification: 2CH
3OH+2NO+1/2O
2→ 2CH
3ONO+H
2O (1-2)
It is that raw material passes through methyl nitrite or ethyl nitrite that above-mentioned research and patent have been established with CO, at Pd/a-Al
2O
3Under the catalyzer, make the processing method of CO oxidation coupling connection generation dimethyl oxalate or oxalic acid diethyl ester, disclose the basic characteristics of such reaction, comprise support of the catalyst and activeconstituents, the basic technology condition of reaction etc.People (CN 85101616) such as Fujian Inst. of Matter Structure, Chinese Academy of Sciences good fortune Chen Geng Shen have also synthesized oxalic acid with similar method gas phase.But these methods all can not be implemented in the cover circulation device and produce dimethyl oxalate coproduction oxalic acid simultaneously or produce oxalic acid diethyl ester coproduction oxalic acid, and the product collection device of these methods all exists bigger technology shortcoming, limited its industrial applications, concrete shortcoming is as follows:
(CN 1056135 in University Of Tianjin, CN 101143821) middle reported method, be oxalic acid diethyl ester to be collected by condenser, its shortcoming is in order to guarantee the processing requirement of circulation gas, the oxalic acid diethyl ester of condenser during almost completely condensation oxonation device is worked off one's feeling vent one's spleen, make the condensation of condenser require very high, therefore need condenser under very low temperature, to move, and need bigger heat interchanging area, cause the condensation energy consumption to increase, the heat-exchange equipment investment increases, even condensing temperature is very low, heat interchanging area is also enough big, still the saturated vapo(u)r that has oxalic acid diethyl ester can enter hydrolysis in the follow-up esterifier like this in gas phase, cause problems such as equipment corrosion.For fear of the barkite hydrolysis equipment is caused corrosion, traditional method is to wash or ethanol mode such as wash is removed barkite in the gas phase by methyl alcohol, if methyl alcohol is washed the problems such as azeotropic that can cause byproduct methylcarbonate and methyl alcohol, ethanol is washed and can be occurred increasing unit equipment equally, increase problems such as separating energy consumption, can increase the product separation cost greatly.
Reported method in the Shanghai Jiaohua Co., Ltd (CN 101190884), be to wash the collection that tower carries out dimethyl oxalate by methyl alcohol, but this method is the physical absorption process, because the restriction of solubleness, need expend a large amount of methyl alcohol, and later separation barkite and methyl alcohol also needs a large amount of separation costs, and the by product methylcarbonate of dimethyl oxalate can form minimum azeotropic mixture with methyl alcohol, cause the separation difficulty when reclaiming methyl alcohol, separation costs is risen greatly.
Reported method in the Fujian Inst. of Matter Structure, Chinese Academy of Sciences (CN 1027257), be to carry out the collection of dimethyl oxalate by condensation methyl alcohol absorption tower, its shortcoming also is because the restriction of solubleness, need expend a large amount of methyl alcohol, and the by product methylcarbonate of dimethyl oxalate can form minimum azeotropic mixture with methyl alcohol, cause the separation difficulty when reclaiming methyl alcohol, separation costs is risen greatly, simultaneously because the condensation absorption, can cause than relatively large nitrous acid ester and be dissolved in the methanol solution of absorption tower still, because nitrous acid ester toxicity is bigger, when reclaiming methyl alcohol, must reclaim its desorb, further increased separation costs again.
People (CN85101616) such as Fujian Inst. of Matter Structure, Chinese Academy of Sciences good fortune Chen Geng Shen are though the gas phase synthesis method of disclosed catalytic synthesis of oxalic acid from carbon monoxide, coupling process can utilize the gas phase synthesis technique to produce high-quality oxalic acid, but because the oxalic acid market capacity is little, and the facility investment of gas phase synthesis method synthesis of oxalic acid is big, so limited its industrially scalable.
The CN1569800 patent disclosure of Shanghai Jiaohua Co., Ltd a kind of method and apparatus of oxalic acid coproduction Sodium Nitrite, this method can obtain the barkite product by esterification column and oxonation device, hydrolysis obtains oxalic acid then.But this patent introduction is a kind of one way route, and the NO that oxonation produces directly absorbs with alkali and obtains Sodium Nitrite, and NO can't recycle; Owing to adopt the one way route, unreacted carbon monoxide and the very difficult recycling of nitrous acid ester completely limited its technology and used during oxonation was worked off one's feeling vent one's spleen in addition.
The utility model content
The purpose of this utility model is to overcome defective of the prior art, and a kind of synthesis of oxalate of suitable large-scale industrialization production and the production system of coproduction oxalic acid are provided.
The utility model is introduced the equipment of condenser and barkite hydrolysis reactor in the CO gas phase coupling synthesis of oxalate circulation process of existing open report, solve many technical problems among the barkite preparation technology with this, and can realize the coproduction of barkite and oxalic acid.
The utility model has adopted following technical proposals:
The production system of a kind of synthesis of oxalate and coproduction oxalic acid comprises gas phase coupling connection oxonation device, first condenser, barkite hydrolysis reactor and esterifier that circulation successively links to each other.
Described barkite hydrolysis reactor can be a tower reactor, also can be tank reactor or the other types reactor that can realize its barkite hydrolysis reaction.
The air outlet of described gas phase coupling connection oxonation device communicates through pipeline with the inlet mouth of first condenser; Described first condenser also is provided with condensation product outlet and air outlet, and the air outlet of first condenser communicates through pipeline with the inlet mouth of barkite hydrolysis reactor; Described barkite hydrolysis reactor also is provided with water-in, liquid outlet and air outlet, and the air outlet of barkite hydrolysis reactor, oxygen blowdown pipe and benefit alcohol pipe (being used for replenishing methyl alcohol or ethanol) all communicate with the import of esterifier through pipeline; Described esterifier also is provided with liquid outlet and air outlet, and the air outlet of esterifier communicates through the inlet mouth of pipeline with gas phase coupling connection oxonation device with the carbon monoxide blowdown pipe.
The pipeline that described esterifier air outlet communicates with the inlet mouth of gas phase coupling connection oxonation device is provided with and discharges a little, is used for speeding by a certain percentage to put circulation gas, to keep the balance of rare gas element ratio in the circulating system.
Preferable, described first condenser is provided with temperature control equipment, so that regulate the ratio of final product barkite and oxalic acid.
Preferable, be connected with second condenser between described barkite hydrolysis reactor and the esterifier, the air outlet of barkite hydrolysis reactor communicates with the inlet mouth of second condenser, the liquid returning tube road that second condenser is provided with condensation product outlet, air outlet and communicates with the barkite hydrolysis reactor, the condensation product outlet of second condenser communicates with the import on esterifier top after pipeline merges with mending pure pipe, and the air outlet of second condenser communicates with the import of esterifier bottom after pipeline merges with the oxygen blowdown pipe.
Preferable, the air outlet of described esterifier communicates with the inlet mouth of the 3rd condenser, the 3rd condenser is provided with phlegma liquid returning tube road and does not coagulate the circulation gas outlet, not coagulating the circulation gas outlet communicates with the inlet mouth of gas phase coupling connection oxonation device, phlegma all returns esterifier, does not coagulate to loop back coupling connection oxonation device after the compressed machine of circulation gas boosts.
The production system of synthesis of oxalate of the present utility model and coproduction oxalic acid can be used for producing dimethyl oxalate or oxalic acid diethyl ester and coproduction oxalic acid.
The beneficial effects of the utility model:
The utility model increases the hydrolysis reactor of condenser and barkite on existing gas-phase synthesis of oxalate flow process or device, owing to be the barkite that utilizes in the hydrolysis reaction absorption circulation gas, belong to chemical absorption, so speed is fast, reactor is little with respect to the pure absorption tower scale of prior art; And because chemical absorption, impellent is big, and specific absorption is more thorough, solved in the circulation gas prior art since condensation thoroughly or because alcohol is washed not thorough, barkite enters the follow-up equipment hydrolysis by gas phase and causes equipment corrosion, energy consumption height, separation costs high-technology problem.
In addition, the utility model utilizes the raw material of the correspondent alcohol of hydrolysis reaction generation in the barkite hydrolysis reactor as esterifier, can also save the original amount that needs the use correspondent alcohol to enter.And the barkite hydrolysis reactor can be designed to the form of reactive distillation, promotes the efficient of hydrolysis reaction, can improve the concentration of correspondent alcohol at the reactive distillation cat head.
The utility model also passes through condenser, most of barkite and carbonic ether are collected with liquid or solid-state form, reduced the separation costs of the barkite solution after the pure absorption, the trace carbon dimethyl phthalate behind the condenser in the circulation gas generates methyl alcohol and CO by hydrolysis reaction
2, avoided forming minimum azeotrope and formed with methyl alcohol, greatly reduce follow-up separating difficulty.Compare existing gas-phase synthesis of oxalate technology, use the utility model can save energy consumption 10～30%.
In addition, in the technical problem of the utility model in solving former barkite synthesis technique, also realized the function of dimethyl oxalate or oxalic acid diethyl ester coproduction oxalic acid, only need the condensing temperature of simple adjustment condenser just can change the gas phase composition of circulation gas medium-height grass acid esters behind the condenser, can change the variant production production allocation of this device barkite and oxalic acid, thereby change the production capacity structure of product more flexibly according to market, make the economic interests maximization.The utility model is compared independent oxalic acid and is prepared production system, has greatly reduced equipment cost especially, utilizes the equipment in the gas-phase synthesis of oxalate, and it is too high to have solved gas phase synthesis technique production oxalic acid cost, the problem of industrialization practical application difficulty.
Description of drawings
Fig. 1 production system synoptic diagram of the present utility model.
Embodiment
The production system of synthesis of oxalate as shown in Figure 1 and coproduction oxalic acid comprises gas phase coupling connection oxonation device 1, first condenser 2, barkite hydrolysis reactor 3 and esterifier 4 that circulation successively links to each other;
Wherein, the inlet mouth 21 of the air outlet, bottom 11 of gas phase coupling connection oxonation device 1 and first condenser 2 communicates through pipeline;
Barkite hydrolysis reactor 3 also is provided with water-in 32, liquid outlet 33 and air outlet 34, and air outlet 34, oxygen blowdown pipe 5 and benefit alcohol pipe 6 (being used for replenishing methyl alcohol or ethanol) communicate with the import 41,42 of esterifier 4 through pipeline;
Further, be connected with second condenser 7 between barkite hydrolysis reactor 3 and the esterifier 4, the air outlet 34 of barkite hydrolysis reactor 3 communicates with the inlet mouth 71 of second condenser, the liquid returning tube road 74 that second condenser 7 is provided with condensation product outlet 72, air outlet 73 and communicates with the barkite hydrolysis reactor, condensation product outlet 72 communicates with esterifier 4 upper inlet 41 after pipeline merges with mending alcohol pipe 6, and air outlet 73 communicates with the lower inlet 42 of esterifier 4 after pipeline merges with oxygen blowdown pipe 5.
Further, the air outlet 44 of described esterifier communicates with the inlet mouth 91 of the 3rd condenser 9, the 3rd condenser is provided with phlegma liquid returning tube road 92 and does not coagulate circulation gas outlet 93, phlegma all returns esterifier, does not coagulate to loop back coupling connection oxonation device after the compressed machine of circulation gas boosts.
The method that the production system of above-mentioned synthesis of oxalate and coproduction oxalic acid is used to produce methyl nitrite or ethyl nitrite and coproduction oxalic acid is as follows:
Circulation gas and the CO that replenishes enter at the top of gas phase coupling connection oxonation device 1 and begin reaction, and the coupling connection generates barkite and small amount of carbon acid esters, and the temperature of coupling connection oxonation device is 120 ℃-150 ℃, and catalyst body is Pd/a-Al
2O
3Reacted gas enters first condenser 2 through gas phase coupling connection oxonation device 1 outlet at bottom pipeline, by changing the temperature of condenser, can change the amount of reaction gas medium-height grass acid esters and carbonic ether condensation, thereby can regulate the production capacity that generates barkite and oxalic acid, the temperature range of the first condenser B is-20 ℃～90 ℃, and pressure range is 0.1MPa～0.5MPa; The barkite and the carbonic ether that are condensed into liquid form or solid form enter barkite product groove district in condenser bottom condensation product outlet 22, and uncooled barkite and carbonic ether gas phase are entered the bottom of barkite hydrolysis reactor 3 with circulation gas, and the water counter current contact that enters with the hydrolysis reactor top, carry out the barkite hydrolysis reaction, generate the alcohol of oxalic acid and corresponding esters, the temperature range of barkite hydrolysis reactor is 25 ℃～98 ℃, and pressure range is 0.1MPa～0.5MPa; The liquid outlet 33 that contains the aqueous solution process barkite hydrolysis reactor 3 of oxalic acid enters follow-up oxalic acid crystallizer and carries out following process, and circulation gas carries second condenser 7 that the pure and mild gas phase water of gas phase enters barkite hydrolysis reactor top, be separated into and do not coagulate circulation gas and aqueous alcoholic solution, the temperature range of second condenser is-5 ℃～5 ℃; Do not coagulate the lower inlet 42 that enters esterifier 4 after circulation gas and the oxygen that replenishes and NO mix, upper inlet 41 by esterifier 4 after aqueous alcoholic solution and the alcohol that replenishes mix enters, and in esterifier 4, carry out esterification, produce nitrous acid ester, the esterifier temperature range is 25 ℃～55 ℃, pressure range is that circulation gas that 0.1MPa～0.5MPa contains nitrous acid ester returns in the gas phase coupling connection oxonation device 1 and reacts, and constitutes a complete circulation loop.Compare conventional gas-phase synthesis of oxalate technology, save energy consumption 10～30%.
This example is a flow process utilizing the production system synthesizing dimethyl oxalate coproduction oxalic acid of synthesis of oxalate of the present utility model and coproduction oxalic acid, and the pressure of all devices is 0.1MPa.The temperature of reaction of gas phase coupling connection oxonation device 1 is 140 ℃, and catalyzer is Pd/a-Al
2O
3, the technological temperature of second condenser 2 is 20 ℃, barkite hydrolysis reactor 3 is designed to reaction fractionating tower in this example, reaction zone temperature is 85 ℃, the temperature of second condenser 7 is-5 ℃, and esterifier 4 also is designed to reaction fractionating tower, and reaction zone temperature is 40 ℃.Under these conditions, dimethyl oxalate output and oxalic acid yield in unit time ratio are: 456: 18.3.The purity of the dimethyl oxalate that obtains through 2 condensations of first condenser is 98.3%, and handling back acquisition purity through rectifying or recrystallization is 99.9% dimethyl oxalate.
Claims (7)
1. the production system of synthesis of oxalate and coproduction oxalic acid is characterized in that, comprising gas phase coupling connection oxonation device, first condenser, barkite hydrolysis reactor and esterifier that circulation successively links to each other.
2. the production system of synthesis of oxalate and coproduction oxalic acid according to claim 1 is characterized in that described barkite hydrolysis reactor is tower reactor or tank reactor.
3. the production system of synthesis of oxalate and coproduction oxalic acid according to claim 1 is characterized in that, the air outlet of described gas phase coupling connection oxonation device communicates through pipeline with the inlet mouth of first condenser; Described first condenser also is provided with condensation product outlet and air outlet, and the air outlet of first condenser communicates through pipeline with the inlet mouth of barkite hydrolysis reactor; Described barkite hydrolysis reactor also is provided with water-in, liquid outlet and air outlet, the air outlet of barkite hydrolysis reactor, oxygen blowdown pipe and be used for replenishing methyl alcohol or alcoholic acid is mended pure Guan Junjing pipeline and communicated with the import of esterifier; Described esterifier also is provided with liquid outlet and air outlet, and the air outlet of esterifier communicates through the inlet mouth of pipeline with gas phase coupling connection oxonation device with the carbon monoxide blowdown pipe.
4. the production system of synthesis of oxalate and coproduction oxalic acid according to claim 1 is characterized in that, the pipeline that described esterifier air outlet communicates with the inlet mouth of gas phase coupling connection oxonation device is provided with and discharges a little.
5. the production system of synthesis of oxalate and coproduction oxalic acid according to claim 1 is characterized in that described first condenser is provided with temperature control equipment.
6. the production system of synthesis of oxalate and coproduction oxalic acid according to claim 1, it is characterized in that, be connected with second condenser between described barkite hydrolysis reactor and the esterifier, the air outlet of barkite hydrolysis reactor communicates with the inlet mouth of second condenser, second condenser is provided with the condensation product outlet, air outlet and the liquid returning tube road that communicates with the barkite hydrolysis reactor, the condensation product outlet of second condenser communicates with the import on esterifier top after pipeline merges with mending pure pipe, and the air outlet of second condenser communicates with the import of esterifier bottom after pipeline merges with the oxygen blowdown pipe.
7. the production system of synthesis of oxalate and coproduction oxalic acid according to claim 1, it is characterized in that, the air outlet of described esterifier communicates with the inlet mouth of the 3rd condenser, the 3rd condenser is provided with phlegma liquid returning tube road and does not coagulate the circulation gas outlet, does not coagulate the circulation gas outlet and communicates with the inlet mouth of gas phase coupling connection oxonation device.
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| CN 200920210195 CN201567298U (en) | 2009-09-25 | 2009-09-25 | Production system for synthesizing oxalic ester and co-producing oxalic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182283A (en) * | 2013-03-21 | 2013-07-03 | 安徽淮化股份有限公司 | NO2 pre-reaction device system used in industrial production of ethylene glycol |
-
2009
- 2009-09-25 CN CN 200920210195 patent/CN201567298U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103182283A (en) * | 2013-03-21 | 2013-07-03 | 安徽淮化股份有限公司 | NO2 pre-reaction device system used in industrial production of ethylene glycol |
| CN103182283B (en) * | 2013-03-21 | 2015-12-23 | 安徽淮化股份有限公司 | NO in ethylene glycol industrial production 2pre-reaction apparatus system |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: SHANGHAI HUAYI ENERGY + CHEMICAL INDUSTRY CO., LTD Free format text: FORMER NAME: SHANGHAI COKING CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 200241 Minhang District, Wu Long Road, No. 4280, Shanghai Patentee after: Shanghai Hua Yi derived energy chemical Co., Ltd Address before: 200241 Minhang District, Wu Long Road, No. 4280, Shanghai Patentee before: Shanghai Coking Co., Ltd. |
|
| CX01 | Expiry of patent term |
Granted publication date: 20100901 |
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| CX01 | Expiry of patent term |