WO2022082723A1 - Method for synthesizing n,n'-diisopropylcarbodiimide by using oxygen as oxidizing agent - Google Patents
Method for synthesizing n,n'-diisopropylcarbodiimide by using oxygen as oxidizing agent Download PDFInfo
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- WO2022082723A1 WO2022082723A1 PCT/CN2020/123225 CN2020123225W WO2022082723A1 WO 2022082723 A1 WO2022082723 A1 WO 2022082723A1 CN 2020123225 W CN2020123225 W CN 2020123225W WO 2022082723 A1 WO2022082723 A1 WO 2022082723A1
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- C07C267/00—Carbodiimides
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- the invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing N,N'-diisopropylcarbodiimide by using oxygen as an oxidant.
- N,N'-Diisopropylcarbodiimide is a good low-temperature biochemical dehydrating agent, used for the synthesis and dehydration of amikacin and amino acids, and also used for acids, anhydrides, aldehydes, ketones, etc. It is also used for the synthesis of peptides and nucleic acids. Used as dehydrating agent or carboxyl activator for polypeptide synthesis, or for coupling of small molecule compounds and polypeptides with carrier proteins. In recent years, the sales situation of DIC has continued to grow, and the supply of products is in short supply.
- Patent CN109485583A discloses a preparation method of N,N'-diisopropylcarbodiimide.
- the method has the following disadvantages: the hydrogen sulfide generated by the reaction has an adverse effect on the environment, and at the same time, it is
- Patent CN103382168A discloses a method for synthesizing N,N'-diisopropylcarbodiimide, comprising the following steps: (1) in an alkaline solution, adding carbon disulfide and isopropylamine, and heating the mixed solution To the set temperature, after the constant temperature reaction for the set time, the mixed solution A is obtained; (2) the mixed solution A and the hydrogen peroxide are mixed and heated to a predetermined temperature, and the mixed solution B is obtained after the constant temperature reaction for a predetermined time; (3) in the alkaline In the environment, the mixed solution B, dichloromethane and isopropylamine are mixed uniformly, then an aqueous sodium hypochlorite solution is added to carry out an oxidation reaction, and N,N'-diisopropylcarbodiimide is obtained by separation and purification.
- the method has the following disadvantages: the reaction steps are complicated and it is difficult to realize industrialized production, and the treatment of a large amount of waste water generated by oxid
- Patent CN108084055A discloses a method for synthesizing N,N'diisopropylcarbodiimide by oxidation of N,N'diisopropylthiourea, firstly using sodium hypochlorite to oxidize dimethylamine to obtain chlorodimethylamine, Then, N,N'diisopropylthiourea is oxidized with chlorodimethylamine under alkaline conditions to obtain N,N'diisopropylcarbodiimide, and the yield is over 93%.
- the method has the following disadvantages: the treatment of a large amount of waste water generated by oxidation is difficult and the production cost is high.
- the object of the present invention is to provide a method for synthesizing N,N' diisopropylcarbodiimide using oxygen as an oxidant, the process steps are safe and reliable, the reaction yield and product purity are high, and it is difficult to handle the large amount of waste salt in the traditional process. question.
- a method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant comprising the following steps:
- Oxygen is introduced, the mass ratio of the N,N' diisopropyl thiourea and oxygen is 1:0.2-0.4, and the oxidation reaction is carried out under the conditions that the control pressure is 5-10MPa and the temperature is 110-120°C 3-4h;
- the mass ratio of the N,N' diisopropylthiourea to the xylene solvent is 1.5:1.
- the amount of MoO 3 or Sb 2 O 4 catalyst in the step 2) is 2% of the amount of the added material.
- the mass ratio of N,N' diisopropylthiourea to oxygen is 1:0.3.
- the pressure of the oxidation reaction in the step 3) is 8MPa and the temperature is 115°C.
- the temperature is lowered to 10°C for suction filtration.
- the present invention has the following advantages:
- the present invention uses oxygen as an oxidant, with high reaction selectivity and low risk, while the amount of waste water produced is greatly reduced and easy to handle, which solves the problem that the amount of waste brine in the traditional process is large and difficult to handle;
- the reaction system is optimized, using MoO 3 or Sb 2 O 4 catalyst, the reaction is carried out in a homogeneous reaction system, which is easy to control and improves the reaction yield.
- the DIC oxidation yield reaches more than 94%, and the purity is 99.5%. above.
- N,N' diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 1.5: 1 , add MoO3 catalyst, The dosage of MoO catalyst is 2 % of the total material amount (ie, the total mass of N,N' diisopropyl thiourea and xylene), and oxygen is introduced, and the mass ratio of N, N' diisopropyl thiourea to oxygen The ratio was 1:0.3, heated to 120°C under 10MPa pressure for 3.5h oxidation reaction, then cooled to 5°C with suction filtration, decolorized and distilled under reduced pressure to obtain DIC. The yield is 94.50%, and the purity is 99.55%. The waste water produced by oxidation can be recycled after passing the test after distillation.
- N,N'diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 1.6: 1 , add MoO3 or Sb 2 O 4 catalyst, the amount of MoO 3 or Sb 2 O 4 catalyst is 3% of the total material amount, and oxygen is introduced, and the mass ratio of N,N' diisopropylthiourea and oxygen is 1:0.4, and the pressure is 5MPa.
- the temperature was raised to 110 °C for 3 hours, and then the temperature was lowered to 10 °C for suction filtration, and DIC was obtained by decolorization and vacuum distillation. The yield is 94.00% and the purity is 99.50%.
- the waste water produced by oxidation can be recycled after being tested and qualified after distillation.
- N,N'diisopropylthiourea into the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 2:1, add Sb 2 O 4 Catalyst, the amount of Sb 2 O 4 catalyst is 1% of the total material amount, oxygen is introduced, the mass ratio of N,N' diisopropylthiourea and oxygen is 1:0.2, and the temperature is raised to 115 ° C under 8MPa pressure. The oxidation reaction was carried out for 4 h, then the temperature was lowered to 15 °C, suction filtration, and DIC was obtained by decolorization and vacuum distillation. The yield is 94.55% and the purity is 99.55%. The waste water produced by oxidation can be recycled after being tested and qualified after distillation.
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Abstract
The present invention relates to a method for synthesizing N,N'-diisopropylcarbodiimide by using oxygen as an oxidizing agent. The method comprises the following steps: adding N,N'-diisopropyl thiourea and a xylene solvent into a high-pressure reaction kettle, wherein the mass ratio of the N,N'-diisopropyl thiourea to the xylene solvent is 1-2 : 1; adding a MoO3 or Sb2O4 catalyst, wherein the amount of the MoO3 or Sb2O4 catalyst is 1-3% of the amount of the added material; introducing oxygen, wherein the mass ratio of N,N'-diisopropyl thiourea to oxygen is 1 : 0.2-0.4; performing an oxidation reaction for 3-4 h under conditions where the pressure is controlled to be 5-10 MPa and the temperature is controlled to be 110-120ºC; and then cooling same to 5-15ºC, suction filtering same, decolorizing same, and distilling same under a reduced pressure to obtain DIC. In the present invention, oxygen is used as an oxidizing agent, the reaction selectivity is high, the risk is low, and at the same time, the amount of waste water produced is greatly reduced and the treatment is easy. In addition, the problem that the amount of waste brine is large and difficult to treat in the traditional process is solved. The method is easy to control, the reaction yield is improved, and the production cost is reduced.
Description
本发明涉及涉及有机化学合成技术领域,具体是一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法。The invention relates to the technical field of organic chemical synthesis, in particular to a method for synthesizing N,N'-diisopropylcarbodiimide by using oxygen as an oxidant.
N,N'-二异丙基碳二亚胺(DIC)是一种很好的低温生化脱水剂,用于阿米卡星及氨基酸的合成脱水,也用于酸、酐、醛、酮等的合成,该品还用于肽、核酸的合成。作为脱水剂或羧基活化剂用于多肽合成,或用于小分子化合物及多肽与载体蛋白的偶联。近年DIC销售形势持续增长,产品供不应求,同时环保压力大,废水处理成为当今难题。N,N'-Diisopropylcarbodiimide (DIC) is a good low-temperature biochemical dehydrating agent, used for the synthesis and dehydration of amikacin and amino acids, and also used for acids, anhydrides, aldehydes, ketones, etc. It is also used for the synthesis of peptides and nucleic acids. Used as dehydrating agent or carboxyl activator for polypeptide synthesis, or for coupling of small molecule compounds and polypeptides with carrier proteins. In recent years, the sales situation of DIC has continued to grow, and the supply of products is in short supply.
目前N,N’-二异丙基碳二亚胺合成的方法主要有以下三种:At present, there are three main methods for the synthesis of N,N'-diisopropylcarbodiimide:
路线1:专利CN109485583A公开了一种N,N’-二异丙基碳二亚胺的制备方法,先用异丙胺和二硫化碳在溶剂中合成N,N’二异丙基硫脲;对N,N’二异丙基硫脲进行抽滤、烘干后进行一次氧化;进行二次氧化反应,加入催化剂和氧化剂,在60-65℃下反应1小时;进行脱硫处理,向氧化液中加入硫化钠溶液,升温至70-75℃,反应1-2小时;加片碱中和,水洗,分去水层,加干燥剂干燥,蒸出溶剂,减压精馏得到N,N’-二异丙基碳二亚胺。该方法存在以下缺点:反应生成的硫化氢对环境造成不利影响,同时氧化生成的大量废盐水处理较为困难。Route 1: Patent CN109485583A discloses a preparation method of N,N'-diisopropylcarbodiimide. First, use isopropylamine and carbon disulfide to synthesize N,N'diisopropylthiourea in a solvent; N'diisopropylthiourea is subjected to suction filtration, drying and then primary oxidation; secondary oxidation reaction is carried out, catalyst and oxidant are added, and the reaction is carried out at 60-65 ° C for 1 hour; Sodium solution, heat up to 70-75°C, and react for 1-2 hours; add a tablet of alkali to neutralize, wash with water, separate the water layer, add desiccant to dry, evaporate the solvent, and rectify under reduced pressure to obtain N,N'-diiso Propylcarbodiimide. The method has the following disadvantages: the hydrogen sulfide generated by the reaction has an adverse effect on the environment, and at the same time, it is difficult to treat a large amount of waste brine generated by oxidation.
路线2:专利CN103382168A 公开了一种N,N’-二异丙基碳二亚胺的合成方法,包括以下步骤:(1)在碱性溶液中,加入二硫化碳和异丙胺,并将混合溶液升温至设定温度,恒温反应设定时间后,得到混合溶液A;(2)将混合溶液A和双氧水混合并升温至预定温度,恒温反应预定时间后,得到混合溶液B;(3)在碱性环境中,将混合溶液B、二氯甲烷和异丙胺混合均匀,然后加入次氯酸钠水溶液进行氧化反应,分离提纯得到N,N’-二异丙基碳二亚胺。该方法存在以下缺点:反应步骤复杂不易实现工业化生产,且氧化生成的大量废水处理较为困难,生产成本高。Route 2: Patent CN103382168A discloses a method for synthesizing N,N'-diisopropylcarbodiimide, comprising the following steps: (1) in an alkaline solution, adding carbon disulfide and isopropylamine, and heating the mixed solution To the set temperature, after the constant temperature reaction for the set time, the mixed solution A is obtained; (2) the mixed solution A and the hydrogen peroxide are mixed and heated to a predetermined temperature, and the mixed solution B is obtained after the constant temperature reaction for a predetermined time; (3) in the alkaline In the environment, the mixed solution B, dichloromethane and isopropylamine are mixed uniformly, then an aqueous sodium hypochlorite solution is added to carry out an oxidation reaction, and N,N'-diisopropylcarbodiimide is obtained by separation and purification. The method has the following disadvantages: the reaction steps are complicated and it is difficult to realize industrialized production, and the treatment of a large amount of waste water generated by oxidation is difficult, and the production cost is high.
路线3:专利CN108084055A公开了一种N,N’二异丙基硫脲氧化合成N,N’二异丙基碳二亚胺的方法,首先使用次氯酸钠氧化二甲胺得到氯代二甲胺,然后在碱性条件下用氯代二甲胺氧化N,N’二异丙基硫脲得到N,N’二异丙基碳二亚胺,收率达到93%以上。该方法存在以下缺点:氧化生成的大量废水处理较为困难,生产成本高。Route 3: Patent CN108084055A discloses a method for synthesizing N,N'diisopropylcarbodiimide by oxidation of N,N'diisopropylthiourea, firstly using sodium hypochlorite to oxidize dimethylamine to obtain chlorodimethylamine, Then, N,N'diisopropylthiourea is oxidized with chlorodimethylamine under alkaline conditions to obtain N,N'diisopropylcarbodiimide, and the yield is over 93%. The method has the following disadvantages: the treatment of a large amount of waste water generated by oxidation is difficult and the production cost is high.
本发明的目的在于提供一种使用氧气作为氧化剂合成N,N’二异丙基碳二亚胺的方法,工艺步骤安全可靠,反应收率及产品纯度高,解决传统工艺废盐水量大难处理问题。The object of the present invention is to provide a method for synthesizing N,N' diisopropylcarbodiimide using oxygen as an oxidant, the process steps are safe and reliable, the reaction yield and product purity are high, and it is difficult to handle the large amount of waste salt in the traditional process. question.
本发明是通过以下技术方案实现的:The present invention is achieved through the following technical solutions:
一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,包括以下步骤:A method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant, comprising the following steps:
1)在高压反应釜中加入N,N’二异丙基硫脲和二甲苯溶剂,所述N,N’二异丙基硫脲和二甲苯溶剂的质量比为1-2:1;1) Add N,N'diisopropylthiourea and xylene solvent into the autoclave, and the mass ratio of the N,N'diisopropylthiourea and xylene solvent is 1-2:1;
2)加入MoO
3或Sb
2O
4催化剂,所述MoO
3或Sb
2O
4催化剂的用量为步骤1中物料总质量的1-3%;
2) Add MoO 3 or Sb 2 O 4 catalyst, and the amount of said MoO 3 or Sb 2 O 4 catalyst is 1-3% of the total mass of the material in step 1;
3)通入氧气,所述N,N’二异丙基硫脲和氧气的质量比为1:0.2-0.4,在控制压力为5-10MPa、温度为110-120℃的条件下进行氧化反应3-4h;3) Oxygen is introduced, the mass ratio of the N,N' diisopropyl thiourea and oxygen is 1:0.2-0.4, and the oxidation reaction is carried out under the conditions that the control pressure is 5-10MPa and the temperature is 110-120°C 3-4h;
4)然后降温至5-15℃抽滤,经脱色、减压蒸馏得到DIC。4) Then the temperature is lowered to 5-15℃, suction filtration, decolorization and vacuum distillation to obtain DIC.
优选的,所述N,N’二异丙基硫脲和二甲苯溶剂的质量比为1.5:1。Preferably, the mass ratio of the N,N' diisopropylthiourea to the xylene solvent is 1.5:1.
优选的,所述步骤2)中MoO
3或Sb
2O
4催化剂的用量为已加入物料量的2%。
Preferably, the amount of MoO 3 or Sb 2 O 4 catalyst in the step 2) is 2% of the amount of the added material.
优选的,所述步骤3)中N,N’二异丙基硫脲和氧气的质量比为1:0.3。Preferably, in the step 3), the mass ratio of N,N' diisopropylthiourea to oxygen is 1:0.3.
优选的,所述步骤3)中氧化反应的压力为8MPa,温度为115℃。Preferably, the pressure of the oxidation reaction in the step 3) is 8MPa and the temperature is 115°C.
优选的,所述步骤4)中降温至10℃抽滤。Preferably, in the step 4), the temperature is lowered to 10°C for suction filtration.
本发明与现有技术相比较,具有以下优点:Compared with the prior art, the present invention has the following advantages:
1、本发明使用氧气作氧化剂,反应选择性高,危险性低,同时废水产生量大幅降低并易于处理,解决了传统工艺废盐水量大难处理问题;1. The present invention uses oxygen as an oxidant, with high reaction selectivity and low risk, while the amount of waste water produced is greatly reduced and easy to handle, which solves the problem that the amount of waste brine in the traditional process is large and difficult to handle;
2、优化了反应体系,使用MoO
3或Sb
2O
4催化剂,使反应在一个均相反应体系中进行,易于控制,提高了反应收率,DIC氧化收率达到94%以上,纯度在99.5%以上。
2. The reaction system is optimized, using MoO 3 or Sb 2 O 4 catalyst, the reaction is carried out in a homogeneous reaction system, which is easy to control and improves the reaction yield. The DIC oxidation yield reaches more than 94%, and the purity is 99.5%. above.
3、工艺步骤绿色环保,并且废水量大幅降低,减少了环保投入,降低了生产成本。3. The process steps are green and environmentally friendly, and the amount of waste water is greatly reduced, which reduces environmental protection investment and reduces production costs.
下面对本发明的实施例作详细说明,本实施例在以本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,但本发明的保护范围不限于下述的实施例。The embodiments of the present invention are described in detail below. This embodiment is implemented on the premise of the technical solution of the present invention, and provides detailed implementation modes and specific operation processes, but the protection scope of the present invention is not limited to the following implementations example.
实施例1Example 1
向高压反应釜中加入N,N’二异丙基硫脲,以二甲苯作溶剂,N,N’二异丙基硫脲和二甲苯溶剂的质量比为1.5:1,加入MoO
3催化剂,MoO
3催化剂的用量为总物料量(即N,N’二异丙基硫脲、二甲苯总质量)的2%,通入氧气,N,N’二异丙基硫脲和氧气的质量比为1:0.3,在10MPa压力下升温至120℃进行氧化反应3.5h,然后降温至5℃抽滤,经脱色、减压蒸馏得到DIC。收率94.50%,纯度99.55%,氧化产生的废水经蒸馏后检测合格后可循环使用。
Add N,N' diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 1.5: 1 , add MoO3 catalyst, The dosage of MoO catalyst is 2 % of the total material amount (ie, the total mass of N,N' diisopropyl thiourea and xylene), and oxygen is introduced, and the mass ratio of N, N' diisopropyl thiourea to oxygen The ratio was 1:0.3, heated to 120°C under 10MPa pressure for 3.5h oxidation reaction, then cooled to 5°C with suction filtration, decolorized and distilled under reduced pressure to obtain DIC. The yield is 94.50%, and the purity is 99.55%. The waste water produced by oxidation can be recycled after passing the test after distillation.
实施例2Example 2
向高压反应釜中加入N,N’二异丙基硫脲,以二甲苯作溶剂,N,N’二异丙基硫脲和二甲苯溶剂的质量比为1.6:1,加入MoO
3或Sb
2O
4催化剂,MoO
3或Sb
2O
4催化剂的用量为总物料量的3%,通入氧气,N,N’二异丙基硫脲和氧气的质量比为1:0.4,在5MPa压力下升温至110℃进行氧化反应3h,然后降温至10℃抽滤,经脱色、减压蒸馏得到DIC。收率94.00%,纯度99.50%,氧化产生的废水经蒸馏后检测合格后可循环使用。
Add N,N'diisopropylthiourea to the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 1.6: 1 , add MoO3 or Sb 2 O 4 catalyst, the amount of MoO 3 or Sb 2 O 4 catalyst is 3% of the total material amount, and oxygen is introduced, and the mass ratio of N,N' diisopropylthiourea and oxygen is 1:0.4, and the pressure is 5MPa. The temperature was raised to 110 °C for 3 hours, and then the temperature was lowered to 10 °C for suction filtration, and DIC was obtained by decolorization and vacuum distillation. The yield is 94.00% and the purity is 99.50%. The waste water produced by oxidation can be recycled after being tested and qualified after distillation.
实施例3Example 3
向高压反应釜中加入N,N’二异丙基硫脲,以二甲苯作溶剂,N,N’二异丙基硫脲和二甲苯溶剂的质量比为2:1,加入Sb
2O
4催化剂,Sb
2O
4催化剂的用量为总物料量的1%,通入氧气,N,N’二异丙基硫脲和氧气的质量比为1:0.2,在8MPa压力下升温至115℃进行氧化反应4h,然后降温至15℃抽滤,经脱色、减压蒸馏得到DIC。收率94.55%,纯度99.55%,氧化产生的废水经蒸馏后检测合格后可循环使用。
Add N,N'diisopropylthiourea into the autoclave, use xylene as solvent, the mass ratio of N,N'diisopropylthiourea and xylene solvent is 2:1, add Sb 2 O 4 Catalyst, the amount of Sb 2 O 4 catalyst is 1% of the total material amount, oxygen is introduced, the mass ratio of N,N' diisopropylthiourea and oxygen is 1:0.2, and the temperature is raised to 115 ° C under 8MPa pressure. The oxidation reaction was carried out for 4 h, then the temperature was lowered to 15 °C, suction filtration, and DIC was obtained by decolorization and vacuum distillation. The yield is 94.55% and the purity is 99.55%. The waste water produced by oxidation can be recycled after being tested and qualified after distillation.
本发明并不限于上述的实施方式,在本领域技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下做出各种变化,变化后的内容仍属于本发明的保护范围。The present invention is not limited to the above-mentioned embodiments, and within the scope of knowledge possessed by those skilled in the art, various changes can also be made without departing from the purpose of the present invention, and the changed content still belongs to the protection scope of the present invention .
Claims (6)
- 一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,其特征在于,包括以下步骤:A method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant, is characterized in that, comprises the following steps:在高压反应釜中加入N,N’二异丙基硫脲和二甲苯溶剂,所述N,N’二异丙基硫脲和二甲苯溶剂的质量比为1-2:1;In the autoclave, add N,N' diisopropyl thiourea and xylene solvent, and the mass ratio of the N, N' diisopropyl thiourea and xylene solvent is 1-2:1;加入MoO 3或Sb 2O 4催化剂,所述MoO 3或Sb 2O 4催化剂的用量为步骤1中物料总质量的1-3%; Add MoO 3 or Sb 2 O 4 catalyst, and the consumption of the MoO 3 or Sb 2 O 4 catalyst is 1-3% of the total mass of the material in step 1;通入氧气,所述N,N’二异丙基硫脲和氧气的质量比为1:0.2-0.4,在控制压力为5-10MPa、温度为110-120℃的条件下进行氧化反应3-4h;Oxygen is introduced, the mass ratio of the N,N' diisopropylthiourea and oxygen is 1:0.2-0.4, and the oxidation reaction is carried out under the condition that the control pressure is 5-10MPa and the temperature is 110-120°C 3- 4h;然后降温至5-15℃抽滤,经脱色、减压蒸馏得到DIC。Then the temperature is lowered to 5-15°C, suction filtration, and DIC is obtained by decolorization and vacuum distillation.
- 根据权利要求1所述的一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,其特征在于:所述N,N’二异丙基硫脲和二甲苯溶剂的质量比为1.5:1。A method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant according to claim 1, it is characterized in that: described N,N'diisopropylthiourea and xylene solvent The mass ratio is 1.5:1.
- 根据权利要求1所述的一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,其特征在于:所述步骤2)中MoO 3或Sb 2O 4催化剂的用量为已加入物料量的2%。 The method for synthesizing N,N' - diisopropylcarbodiimide using oxygen as an oxidant according to claim 1 , wherein the amount of MoO3 or Sb2O4 catalyst in the step 2 ) is used 2% of the added material.
- 根据权利要求1所述的一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,其特征在于:所述步骤3)中N,N’二异丙基硫脲和氧气的质量比为1:0.3。A method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant according to claim 1, characterized in that: in the step 3), N,N'diisopropylthiourea The mass ratio of oxygen and oxygen is 1:0.3.
- 根据权利要求1所述的一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,其特征在于:所述步骤3)中氧化反应的压力为8MPa,温度为115℃。A method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant according to claim 1, wherein the pressure of the oxidation reaction in the step 3) is 8MPa, and the temperature is 115 °C.
- 根据权利要求1所述的一种使用氧气作为氧化剂合成N,N'-二异丙基碳二亚胺的方法,其特征在于:所述步骤4)中降温至10℃抽滤。A method for synthesizing N,N'-diisopropylcarbodiimide using oxygen as an oxidant according to claim 1, characterized in that: in the step 4), the temperature is lowered to 10°C for suction filtration.
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