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Preparation method for bromoalkane

A bromoalkane and crude product technology, which is applied in the field of bromoalkane preparation, can solve problems such as troublesome post-processing, complex catalyst synthesis and regeneration process affecting popularization, unstable yield of bromoalkane, etc., to achieve good product quality and production The effect of low cost and stable product quality

Inactive Publication Date: 2012-12-19
SHANDONG TIANYI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The sulfuric acid catalyst method will produce a large amount of dilute sulfuric acid in the production process, and the post-treatment is relatively troublesome; the solid acid catalysis method is easily affected by the catalyst failure process, resulting in unstable yield of brominated alkanes, and the complex synthesis and regeneration process of the catalyst affects the production process. promotion of craftsmanship

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  • Preparation method for bromoalkane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 向450Kg 浓度为48%的氢溴酸中加入92 Kg无水乙醇,搅拌25分钟,生成混合料液,搅拌下加热混合料液达到回流状态,保持搅拌和回流状态使物料反应10小时,制得产物混合液A;在37-42℃温度条件下蒸馏产物混合液A,蒸出的气体经冷凝后制得产物混合液B;将产物混合液B静置35分钟使之分层,取下层液体制得溴乙烷粗品C 198.4公斤;向上述溴乙烷粗品C中加入200升水与50升4%的碳酸钠溶液,然后搅拌洗涤30分钟,得pH值为7.5的洗涤混合液,静置洗涤混合液使之分层,取出下层的液体得溴乙烷粗品D 188.3公斤,将溴乙烷粗品D加入到精馏塔中在温度38-41℃条件下进行精馏,蒸出的气体经冷凝后,便得到液体状的溴乙烷182.03公斤,按乙醇计收率为83.5%,溴乙烷的主含99.93%。

Embodiment 2

[0024] 向422Kg 浓度为48%的氢溴酸中加入60Kg无水正丙醇,搅拌35分钟,生成混合料液,搅拌下加热混合料液达到回流状态,保持搅拌和回流状态使物料反应12小时,制得产物混合液A;在71-76℃温度条件下蒸馏产物混合液A,蒸出的气体经冷凝后制得产物混合液B;将产物混合液B静置30分钟使之分层,取下层液体制得溴代正丙烷粗品C 114.4公斤;向上述溴代正丙烷粗品C中加入200升水与20升5%的碳酸钠溶液,然后搅拌洗涤30分钟,得pH值为8.1的洗涤混合液,静置洗涤混合液使之分层,取出下层的液体得溴代正丙烷粗品D 109公斤,将溴代正丙烷粗品D加入到精馏塔中在温度72-75℃条件下进行精馏,蒸出的气体经冷凝后,便得到液体状的溴代正丙烷104.66公斤,按正丙醇计收率为85.1%,溴代正丙烷的主含99.92%。

Embodiment 3

[0026] 向608Kg 浓度为48%的氢溴酸中加入60Kg无水异丙醇,搅拌30分钟,生成混合料液,搅拌下加热混合料液达到回流状态,保持搅拌和回流状态使物料反应12小时,制得产物混合液A;在58-63℃温度条件下蒸馏产物混合液A,蒸出的气体经冷凝后制得产物混合液B;将产物混合液B静置30分钟使之分层,取下层液体制得溴代异丙烷粗品C113.2公斤;向上述溴代异丙烷粗品C中加入200升水与30升5%的碳酸钠溶液,然后搅拌洗涤30分钟,得pH值为8.2的洗涤混合液,静置洗涤混合液使之分层,取出下层的液体得溴代异丙烷粗品D109.3公斤,将溴代异丙烷粗品D加入到精馏塔中在温度59-62℃条件下进行精馏,蒸出的气体经冷凝后,便得到液体状的溴代异丙烷106.08公斤,按异丙醇计收率为86.2%,溴代异丙烷的主含99.93%。

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Abstract

The invention discloses a preparation method for bromoalkane. The preparation method comprises the following steps of: mixing lower alcohol with hydrobromic acid; heating a mixture to a reflow state; enabling the lower alcohol and the hydrobromic acid in the mixture to fully react to obtain a product mixed solution A; distilling the product mixed solution A; condensing the distilled gas to obtain a product mixed solution B; standing the product mixed solution B for layering; taking a lower-layer liquid to obtain a bromoalkane crude product C; rectifying the bromoalkane crude product C; and condensing the rectified gas to obtain liquid bromoalkane. The preparation method has the advantages of simplicity in process and reaction control, no need of catalyst, low production cost, less pollution, favorable quality of products and high purity.

Description

technical field [0001] 本发明涉及一种溴代烷的制备方法。 Background technique [0002] 以溴化氢或氢溴酸为主要原料制备的溴代烷是精细化工领域的后起之秀,广泛应用在医药、农药、染料、香料、阻燃、灭火、合成材料、电子刻蚀等领域,发挥着无可替代的作用,具有广阔的市场前景和良好的经济效益。 [0003] 目前溴代烷的合成主要有醇与溴化钠硫酸法、醇与氢溴酸法、醇与溴素硫磺法等方法为主,但是醇溴化钠硫酸法、醇溴素硫磺法等工艺均系间歇法生产、副产大量的稀硫酸,设备的利用率低,环保处理相对复杂。另外氢溴酸和醇在催化剂存在的条件下反应生产溴代烷,由于氢溴酸作为大量生产芳基溴化物阻燃剂的副产物,经济上合理,是近几年研究的热点。此种方法在合成过程中需要添加适当的催化剂,根据催化剂的不同可以分为两大类,一类是硫酸法,一类是固体超强酸法。硫酸催化剂法在生产过程中会产生大量的稀硫酸,后处理相对麻烦;固体酸催化法易受催化剂失效过程的影响而导致溴代烷收率不稳定,同时催化剂合成与再生过程复杂影响了该工艺的推广。 Contents of the invention [0004] 本发明的目的是提供一种溴代烷的制备方法。 [0005] 为了达到上述发明目的,本发明采用的第一种技术方案包含以下步骤: [0006] (1)按低碳醇与HBr的摩尔比为1:1-5的配比关系将低碳醇与氢溴酸混合制得混合料液;加热混合料液达到回流状态,保持回流状态直至物料充分反应,制得产物混合液A; [0007] (2)蒸馏产物混合液A,蒸出的气体经冷凝后制得产物混合液B;静置产物混合液B使之分层,取下层液体制得溴代烷粗品C; [0008] (3)精馏溴代烷粗品C,蒸出的气体经冷凝后便制得液体状的溴代烷。 [0009] 所述溴代烷粗品C在精馏之前还需经碱液洗涤的步骤;即向溴代烷粗品C中加入碱液对溴代烷粗品C进行洗涤,以获得pH值大于等于6的洗涤混合液,静置洗涤混合液使之分层,取出下层的液体得溴代烷粗品D,将溴代烷粗品D进行精馏,蒸出的气体经冷凝后便制得液体状的溴代烷。 [0010] 上述技术方案中,所述碱液为碱的水溶液,碱的用量为溴代烷粗品C质量的0.025-0.5倍,水的用量为溴代烷粗品C质量的0.5-2....

Claims

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Application Information

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IPC IPC(8): C07C19/075C07C17/16
Inventor 唐星三孟烨李茂桉孙跃明孙广志董勇张军
Owner SHANDONG TIANYI CHEM
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