WO2022120615A1 - 一种富马酸生产工艺 - Google Patents
一种富马酸生产工艺 Download PDFInfo
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- WO2022120615A1 WO2022120615A1 PCT/CN2020/134733 CN2020134733W WO2022120615A1 WO 2022120615 A1 WO2022120615 A1 WO 2022120615A1 CN 2020134733 W CN2020134733 W CN 2020134733W WO 2022120615 A1 WO2022120615 A1 WO 2022120615A1
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- Prior art keywords
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- fumaric acid
- same
- room temperature
- reactor
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- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 title claims abstract description 38
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000001530 fumaric acid Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000007710 freezing Methods 0.000 claims abstract description 12
- 230000008014 freezing Effects 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims abstract description 8
- 235000019838 diammonium phosphate Nutrition 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 38
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 5
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 5
- 239000011976 maleic acid Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000004042 decolorization Methods 0.000 claims description 4
- 230000002045 lasting effect Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 238000001914 filtration Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 229910017053 inorganic salt Inorganic materials 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000004383 yellowing Methods 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/353—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by isomerisation; by change of size of the carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C57/00—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms
- C07C57/02—Unsaturated compounds having carboxyl groups bound to acyclic carbon atoms with only carbon-to-carbon double bonds as unsaturation
- C07C57/13—Dicarboxylic acids
- C07C57/15—Fumaric acid
Definitions
- the invention relates to the technical field of fumaric acid production, in particular to a fumaric acid production process.
- Fumaric acid is a colorless, flammable crystalline, carboxylic acid derived from butene.
- the traditional catalyst used is organic compound-thiourea, and a certain amount of sulfuric acid is added in the actual reaction process to improve its catalytic activity, which causes serious corrosion to equipment, and the obtained finished product is rich in
- the color of maleic acid is yellow, and the thiourea in the production wastewater is difficult to degrade, which brings great difficulty to the subsequent treatment and discharge of the wastewater.
- the purpose of the present invention is to propose a fumaric acid production process and its preparation method in order to solve the shortcomings existing in the prior art.
- a fumaric acid production process comprising the following steps:
- the solution A in the reactor is subjected to freezing treatment, and the reactor is heated after the freezing, when the solution temperature in the reactor is at 45 °C-50 °C, add urea and continue stirring to obtain solution B;
- the stirring speed in S3 is 100 rpm.
- the stirring time in S3 is 2 hours.
- the decolorization treatment time in S1 is 45min.
- the present invention uses urea as a catalyst, and can neutralize the urea through diammonium hydrogen phosphate during use to form inorganic salt components, so that the residual waste liquid is less polluted, and does not need to be degraded. After treatment, it can be discharged and decolorized by activated carbon. The product is pure white and will not turn yellow.
- a kind of fumaric acid production process provided by the invention comprises the following steps:
- the maleic acid aqueous solution is decolorized with activated carbon, and the time of decolorization is 45min to obtain solution A.
- a kind of fumaric acid production process provided by the invention comprises the following steps:
- the maleic acid aqueous solution is decolorized with activated carbon, and the time of decolorization is 45min to obtain solution A.
- the invention uses urea as a catalyst, and can neutralize the urea through diammonium hydrogen phosphate during use to form inorganic salt components, so that the residual waste liquid is less polluted, does not need to be degraded, and can be discharged after simple treatment , Decolorized by activated carbon, the product is pure white and will not turn yellow.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
提供了一种富马酸生产工艺,包括以下步骤:采用活性炭进行脱色处理,过滤后加入反应釜;进行冷冻处理,冷冻后对反应釜进行加热,加入尿素并持续搅拌;保持50℃并持续一小时,停止加热并自然冷却,持续降温至-6℃并保持15min;在室温下自动升温,加入磷酸氢二铵,再次加热至77℃,自然状态下冷却,当反应釜内温度降至室温后,离心得到富马酸。所述方法通过尿素作为催化剂,且使用过程中通过磷酸氢二铵对尿素进行中和,形成无机盐成分,残余的废液污染小,无需对其进行降解,简单的处理后即可进行排放,通过活性炭进行脱色处理,产品为纯白色,不会发黄。
Description
本发明涉及富马酸生产技术领域,尤其涉及一种富马酸生产工艺。
富马酸是一种无色、易燃的晶体,由丁烯衍生出的羧酸。目前在生产富马酸的工艺中,传统使用的催化剂是有机化合物-硫脲,并且在实际反应过程中还要加入一定量的硫酸以提高其催化活性,对设备腐蚀较为严重,得到的成品富马酸颜色发黄,且生产废水中的硫脲难以降解,给废水的后续处理及排放带来较大难度。
发明内容
本发明的目的是为了解决现有技术中存在的缺点,而提出的一种富马酸生产工艺及其制备方法。
为了实现上述目的,本发明采用了如下技术方案:
一种富马酸生产工艺,包括以下步骤:
S1、将顺丁烯二酸水溶液采用活性炭进行脱色处理,得到溶液A;
S2、将溶液A过滤后加入反应釜;
S3、对反应釜内的溶液A进行冷冻处理,冷冻后对反应釜进行加热,当反应釜内的溶液温度在45℃-50℃时加入尿素并持续搅拌得到溶液B;
S4、将溶液B保持45℃-50℃并持续一小时,停止加热并自然冷却, 当溶液B冷却至35℃时,对溶液B持续降温至-6℃并保持15min;
S5、将S4降温后的溶液B在室温下自动升温,当恢复室温后,加入磷酸氢二铵,再次加热至65℃-70℃,保持此温度反应25min,再次加热至75℃-80℃,持续一小时后自然状态下冷却,当反应釜内温度降至室温后,离心得到富马酸。
优选地,在S3中搅拌的转速为100转/分钟。
优选地,在S3中搅拌的时间为2小时。
优选地,S1中脱色处理的时间为45min。
本发明的优点在于:本发明通过尿素作为催化剂,且使用过程中能够通过磷酸氢二铵对尿素进行中和,形成无机盐成分,这样残余的废液污染小,无需对其进行降解,简单的处理后即可进行排放,通过活性炭进行脱色处理,产品为纯白色,不会发黄。
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
实施例1
本发明提供的一种富马酸生产工艺,包括以下步骤:
S1、将顺丁烯二酸水溶液采用活性炭进行脱色处理,脱色处理的时间为45min,得到溶液A。
S2、将溶液A进行过滤,出去杂质与活性炭,过滤后加入反应釜。
S3、对反应釜内的溶液A进行冷冻处理,冷冻后能够观察到是否过滤干净且有利于后续的反应进行,冷冻后对反应釜进行加热,当反应釜内的溶液温度在50℃时加入尿素并持续搅拌得到溶液B,搅拌的转速为100转/分钟,搅拌的时间为2小时。
S4、将溶液B保持50℃并持续一小时,停止加热并自然冷却,当溶液B冷却至35℃时,对溶液B持续降温至-6℃并保持15min,这样方便后续结晶,更容易与磷酸氢二铵充分反应。
S5、将S4降温后的溶液B在室温下自动升温,当恢复室温后,加入磷酸氢二铵,再次加热至68℃,保持此温度反应25min,再次加热至77℃,持续一小时后自然状态下冷却,当反应釜内温度降至室温后,离心得到富马酸。
实施例2
本发明提供的一种富马酸生产工艺,包括以下步骤:
S1、将顺丁烯二酸水溶液采用活性炭进行脱色处理,脱色处理的时间为45min,得到溶液A。
S2、将溶液A进行过滤,出去杂质与活性炭,过滤后加入反应釜。
S3、对反应釜内的溶液A进行冷冻处理,冷冻后能够观察到是否过滤干净且有利于后续的反应进行,冷冻后对反应釜进行加热,当反应釜内的溶液温度在50℃时加入尿素并持续搅拌得到溶液B,搅拌的转速为100转/分钟,搅拌的时间为2小时。
S4、将溶液B保持48℃并持续一小时,停止加热并自然冷却,当溶液B冷却至35℃时,对溶液B持续降温至-6℃并保持15min,这样方便后续结晶,更容易与磷酸氢二铵充分反应。
S5、将S4降温后的溶液B在室温下自动升温,当恢复室温后,加入磷酸氢二铵,再次加热至678℃,保持此温度反应25min,再次加热至78℃,持续一小时后自然状态下冷却,当反应釜内温度降至室温后,离心得到富马酸。
本发明通过尿素作为催化剂,且使用过程中能够通过磷酸氢二铵对尿素进行中和,形成无机盐成分,这样残余的废液污染小,无需对其进行降解,简单的处理后即可进行排放,通过活性炭进行脱色处理,产品为纯白色,不会发黄。
以上显示和描述了本发明的基本原理、主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的仅为本发明的优选例,并不用来限制本发明,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (4)
- 一种富马酸生产工艺,其特征在于,包括以下步骤:S1、将顺丁烯二酸水溶液采用活性炭进行脱色处理,得到溶液A;S2、将溶液A过滤后加入反应釜;S3、对反应釜内的溶液A进行冷冻处理,冷冻后对反应釜进行加热,当反应釜内的溶液温度在45℃-50℃时加入尿素并持续搅拌得到溶液B;S4、将溶液B保持45℃-50℃并持续一小时,停止加热并自然冷却,当溶液B冷却至35℃时,对溶液B持续降温至-6℃并保持15min;S5、将S4降温后的溶液B在室温下自动升温,当恢复室温后,加入磷酸氢二铵,再次加热至65℃-70℃,保持此温度反应25min,再次加热至75℃-80℃,持续一小时后自然状态下冷却,当反应釜内温度降至室温后,离心得到富马酸。
- 根据权利要求1所述的一种富马酸生产工艺,其特征在于:在S3中搅拌的转速为100转/分钟。
- 根据权利要求1所述的一种富马酸生产工艺,其特征在于:在S3中搅拌的时间为2小时。
- 根据权利要求1所述的一种富马酸生产工艺,其特征在于:S1中脱色处理的时间为45min。
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Cited By (1)
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CN115554835A (zh) * | 2022-11-23 | 2023-01-03 | 佳诺威集团股份有限公司 | 一种纤维板制胶反应釜尾气处理系统 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2207915A (en) * | 1985-02-05 | 1989-02-15 | Nitrokemia Ipartelepek | Preparation of pure fumaric acid |
CN101781188A (zh) * | 2010-02-26 | 2010-07-21 | 镇江市联港化学科技有限公司 | 富马酸的生产方法 |
CN102432456A (zh) * | 2010-09-29 | 2012-05-02 | 烟台恒源生物工程有限公司 | 富马酸的合成方法 |
CN104045550A (zh) * | 2013-11-29 | 2014-09-17 | 淮北晶源生物工程有限责任公司 | 一种富马酸生产工艺 |
-
2020
- 2020-12-09 WO PCT/CN2020/134733 patent/WO2022120615A1/zh active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
GB2207915A (en) * | 1985-02-05 | 1989-02-15 | Nitrokemia Ipartelepek | Preparation of pure fumaric acid |
CN101781188A (zh) * | 2010-02-26 | 2010-07-21 | 镇江市联港化学科技有限公司 | 富马酸的生产方法 |
CN102432456A (zh) * | 2010-09-29 | 2012-05-02 | 烟台恒源生物工程有限公司 | 富马酸的合成方法 |
CN104045550A (zh) * | 2013-11-29 | 2014-09-17 | 淮北晶源生物工程有限责任公司 | 一种富马酸生产工艺 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115554835A (zh) * | 2022-11-23 | 2023-01-03 | 佳诺威集团股份有限公司 | 一种纤维板制胶反应釜尾气处理系统 |
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