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Method for preparing methyl carbamate by urea alcoholysis method and device thereof

A technology for methyl carbamate and a preparation device, applied in the field of synthesizing methyl carbamate, can solve the problems of increased environmental burden, phosgene is highly toxic, and chlorine is difficult to remove, and achieves reduced production cost, easy operation, and safe production process. Effect

Active Publication Date: 2017-05-10
中榆化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This production process has many processes, complex equipment, and the most corrosive hydrochloric acid produced in the production process. The residual chlorine in the product is difficult to remove, the environmental burden increases, and phosgene is highly toxic. It has been gradually replaced by non-phosgene methods. , the production of methyl carbamate from urea and methanol is the most representative non-phosgene method

Method used

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  • Method for preparing methyl carbamate by urea alcoholysis method and device thereof
  • Method for preparing methyl carbamate by urea alcoholysis method and device thereof

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preparation example Construction

[0029] The preparation process of the above catalyst includes the following steps:

[0030] Step 1. Put the silicon oxide into the hydrochloric acid solution, nitric acid solution or acetic acid solution, and then place it at 20-60℃, 0.1-0.3MPa and stir for 12-28h, and then at 120-180℃, Aging for 15-28h; a solid carrier is obtained.

[0031] Step 2: Add the active component and the auxiliary metal to the distilled water, and the solution will be obtained after stirring evenly; wherein the mass ratio of the active component and the auxiliary metal is 1:0.1-1; and the active components are Mg, Ca, Zn, At least one hydrochloride, nitrate or acetate among Fe, Cu or Pb; wherein the auxiliary metal is at least one of La, K, Sr or Ce.

[0032] Step 3. Add the solution obtained in step 2 to the solid carrier obtained in step 1, heat it to 30-80°C, stir for 8-18h; then dry it at 60-130°C for 5-10h; After calcination at -500°C for 2-8 hours, a catalyst for preparing methyl carbamate is obtai...

Embodiment 1

[0040] The specific process of preparing methyl carbamate is:

[0041] First prepare the catalyst: select silicon oxide for pretreatment, put the silicon oxide into the constant temperature zone of the quartz reactor, heat up to 40°C, add hydrochloric acid under normal pressure, and keep stirring for 14 hours, and then place it at 125°C. Store and age for 18 hours, and finally filter to obtain a solid carrier. Add 1.0g of Pb(C 2 H 3 O 2 ) 2 , 0.5g of ZnCl 2 , 0.5g of CaCl 2 Add 0.1g of La and 0.1g of Sr to distilled water and stir evenly to obtain a solution. The above solution was poured into 100.0 g of the treated silica carrier, and then heated to 40°C and stirred for 12 hours, then placed in an oven, dried at 80°C for 8 hours; finally, calcined at 450°C for 6 hours to obtain the catalyst.

[0042] Then weigh 10 g of urea, measure 40 mL of methanol, put it into the reaction kettle, and add 1.5 g of the above-mentioned catalyst, and heat rapidly from room temperature to 140° C. ...

Embodiment 2

[0044] The specific process of preparing methyl carbamate is:

[0045] First prepare the catalyst: select silicon oxide for pretreatment, put the silicon oxide into the constant temperature zone of the quartz reactor, heat up to 40°C, add acetic acid under normal pressure, keep stirring for 12 hours, and then place it at 120°C. Store and age for 16 hours, and finally filter to obtain a solid carrier. Add 0.5g of Pb(NO 3 ) 2 , 0.5g of ZnCl 2 , 0.5g of CuCl 2 Add 0.1 g of La and 0.2 g of Ce into distilled water and stir evenly to obtain a solution. The above solution was poured into 105.0 g of the treated silica support, and then heated to 40°C and stirred for 10 hours, then placed in an oven, dried at 80°C for 6 hours; finally, calcined at 400°C for 5 hours to obtain the catalyst.

[0046] Then weigh 10 g of urea, measure 40 mL of methanol, put it into the reactor, and add 2.0 g of the above-mentioned catalyst. Under magnetic stirring, it will be rapidly heated from room temperatur...

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Abstract

The invention discloses a method for preparing methyl carbamate by a urea alcoholysis method and a device thereof. The method comprises the steps that urea and methanol are mixed; then, a catalyst is added; the temperature is raised to 120 to 200 DEG C; reaction is performed for 0.8 to 8h; the temperature is lowered to room temperature; after filtering and separation, the methyl carbamate is obtained; the catalyst comprises 0.1 to 12 mass percent of active ingredients, 0.1 to 10 mass percent of auxiliary agent metal and the balance silicon oxide; the active ingredients are at least one of hydrochloride, nitrate or acetate of Mg, Ca, Zn, Fe, Cu or Pb; the auxiliary agent metal is at least one of La, K, Sr or Ce. The catalyst can be used for preparing the methyl carbamate by the urea alcoholysis method; the environment pollution cannot be caused; the process is simple; the large-scale production is easy; meanwhile, the preparation device can realize the industrialization of preparation of the methyl carbamate by the urea alcoholysis method.

Description

Technical field [0001] The invention belongs to the technical field of synthetic methyl carbamate, and relates to a method for preparing methyl carbamate by using a urea alcoholysis method. It also relates to the above-mentioned apparatus for preparing methyl carbamate. Background technique [0002] Methyl carbamate is a typical carbamate compound and an important green fine chemical raw material. It has a wide range of uses. It can be used in pesticides, medicine, synthetic resin modification and organic synthesis intermediates, such as: It can be used to synthesize isocyanates, non-toxic polyurethanes, melamine derivatives, and polyvinylamines, and react with unsaturated hydrocarbons, aldehydes and ketones, polyols, and aromatic rings to generate derivatives for various purposes. It can also be used to synthesize heterocyclic pyrroles, three Compounds such as oxazolone, quinazolinone and triazine. In addition, methyl carbamate can also be used as a clothing insect repellent a...

Claims

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Application Information

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IPC IPC(8): C07C269/00C07C271/12B01J23/14B01J23/835B01J23/83B01J23/78B01J23/10
CPCB01J23/10B01J23/14B01J23/78B01J23/83B01J23/835C07C269/00C07C271/12
Inventor 姚建亮
Owner 中榆化工科技有限公司
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