Preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid

A technology of cyanuric acid and materials, which is applied in the field of preparation of high-yield cyanuric acid and its dichloro and trichloro derivatives, achieves the effects of less side reactions, rapid production and solving adhesion problems

Active Publication Date: 2012-06-27
河北田加力生物科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is also to provide a preparation method of derivative sodium dichloroisocyanurate and trichloroisocyanuric acid of cyanuric acid, which can solve the problem of adhesion on the heating surface during product preparation, And make the production fast and continuous, so as to improve the efficiency of industrial production

Method used

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  • Preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid

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Experimental program
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Effect test

Embodiment 1

[0016] Embodiment 1: (high yield) The preparation method of cyanuric acid is to make cyanuric acid product through the following process steps in sequence (see the following reaction formula):

[0017]

[0018] ①Mix 1500 kg of urea and 150 kg of catalyst ammonium sulfate in the mixer according to the weight ratio of 1:0.1 (the mixing of urea and catalyst ammonium sulfate should be uniform to reduce the occurrence of side reactions of urea), and mix them Add it into a (2000 liters) reactor with a heat transfer oil circulation heating method, and start stirring. ② Control the temperature of the heat-conducting oil in the jacket of the reaction kettle to 190°C, open the jacket valve, feed hot oil, and heat up the material. The material will gradually melt at 80-90°C (at 90°C, it will become a slurry liquid). As the temperature rises to 110-130°C (120°C in this embodiment), the material becomes a clear liquid (clarified liquid). ③When the material is completely melted, continu...

Embodiment 2

[0019] Embodiment 2: (high yield) The preparation method of cyanuric acid is to make the cyanuric acid product through the following process steps successively:

[0020] ①Mix 1,500 kg of urea and 300 kg (or 200 kg) of catalyst ammonium sulfate in a mixer evenly (the mixture of urea and catalyst ammonium sulfate should be uniform to reduce the side reactions of urea), and add it to the In the oil circulation heating method (2000 liters) reactor, start stirring. ② Control the temperature of the heat transfer oil in the jacket of the reaction kettle to 150°C (or 175°C), open the jacket valve, feed hot oil, and heat up the material. The material will gradually melt at 80-90°C (90°C becomes slurry liquid). As the temperature rises to 110-130°C (125°C in this embodiment), the material becomes a clear liquid (clarified liquid). ③When the material is completely melted, continue to heat up, and when the temperature rises to 180°C, the material begins to become turbid and appear milky...

Embodiment 3

[0021] Embodiment 3: the preparation method of the derivant sodium dichloroisocyanurate of cyanuric acid is to make the sodium dichloroisocyanurate product (referring to the following reaction formula) through the following process steps successively:

[0022]

[0023] Step 1., 2., 3., 4., 5., 6. are the same as embodiment 1. Step ⑦ is to directly produce its derivative sodium dichloroisocyanurate according to the conventional method without drying the high-quality wet material cyanuric acid, and finally obtain the sodium dichloroisocyanurate product (finished product). Specifically, 1000 kilograms of the wet material cyanuric acid refined product obtained in Example 1 or the present example was added to a 5000-liter reactor, which was equivalent to 6.2 kmol in pure form. Add 1800 kg (12.4 kmol) of NaOH solution with a concentration of 30% by weight, stir and heat up to 40°C, all the materials are dissolved, and a light yellow transparent solution is obtained. Cool down to...

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Abstract

A preparation method of high-yield cyanuric acid and its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid comprises the following steps of: uniformly mixing urea and a catalyst ammonium sulfate, adding the mixture into a reaction vessel, forming a uniform thin material layer on a conveyor belt when the materials reach a certain temperature, liquid viscosity is increased and the liquid is still at a liquid state, and allowing the thin material layer to pass through a tunnel type heating chamber of a tunnel type heating device for heating at high temperature such that the temperature of the materials is rapidly raised to 250-280 DEG C in a short time. As the reaction time of the materials is short and the reaction speed is fast, there are few side effects and product decomposition is low. The cyanuric acid crude product prepared in the invention has high purity and high yield. During the refining process, inorganic dilute acid is used to process the cyanuric acid crude product. After centrifugation, a cyanuric acid refined product is directly used in the synthesis of its derivatives sodium dichloroisocyanurate and trichloroisocyanuric acid without being dried. By the adoption of the method, the adhesive problem of heating surface in production preparation is solved, production speediness and continuity are realized, and industrial production efficiency is raised.

Description

technical field [0001] The present invention relates to a kind of preparation method of cyanuric acid, the present invention also relates to the preparation method of the derivative sodium dichloroisocyanurate of cyanuric acid and trichloroisocyanuric acid, belong to the preparation field of chemical raw material intermediate, generally speaking is a A preparation method of high-yield cyanuric acid and its dichloro and trichloro derivatives. Background technique [0002] Cyanuric acid is an intermediate of organic chemical raw materials. It is widely used. It is mainly used in the preparation of cyanuric acid chloride, salts, esters, bleaching agents, resins, antioxidants, paints, selective herbicides and metals. The synthesis of cyanide moderators, as well as additives for nylon, plastic flame retardants and cosmetics, plays an important role in organic synthesis. There are many methods for the synthesis of cyanuric acid, such as cyanuric acid polymerization, cyanuric acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/32C07D251/36
Inventor 黄诘李志新杨勇卜广伟
Owner 河北田加力生物科技股份有限公司
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