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Continuous 3-methyl-3-buten-1-ol production method

A technology of butene and methyl, applied in the field of organic chemical industry, can solve the problems of low heat and mass transfer efficiency, low production efficiency, and high reaction pressure, and achieve the advantages of avoiding formaldehyde residue, improving conversion rate, and reducing reaction temperature and reaction time. Effect

Active Publication Date: 2016-06-22
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] The purpose of the present invention is to provide a complete set of process schemes for continuous production of 3-methyl-3-buten-1-ol, to solve the problems of low heat and mass transfer efficiency, high reaction pressure, many side reactions, and low production efficiency in the batch process. Low-level deficiencies, realize the continuous production of 3-methyl-3-buten-1-ol with isobutylene and formaldehyde hemiacetal as raw materials

Method used

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  • Continuous 3-methyl-3-buten-1-ol production method

Examples

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Effect test

Embodiment 1

[0032] use figure 1 The shown continuous reaction device carries out the following operation process. Add 100kg of paraformaldehyde and 450L of industrial sodium methoxide solution (3%) to the depolymerization kettle 2 in which paraformaldehyde is dissolved, heat to 40°C while stirring, continue stirring for 1h until the paraformaldehyde is completely dissolved, and then undergo heat exchange respectively 5 and 6, the materials are preheated, and the isobutene and formaldehyde hemiacetal are fed into the tubular reactor 8 with a molar ratio of 4:1, and the feeding space velocity is maintained for 1.2h -1 , maintain the reaction temperature at 170-180°C, the reaction pressure at 9-10MPa, and continue to react for 25 hours. Then the material enters the isobutene recovery tower 10, and the separated isobutene is cooled at -10--15°C and recovered to the isobutene storage tank. Light tower 11, methanol is separated for recycling, the bottom material flows into the product refining...

Embodiment 2

[0034] use figure 1 The shown continuous reaction device carries out the following operation process. Add 50 kg of paraformaldehyde and 220 L of industrial sodium methoxide solution (4%) to the depolymerization kettle 2 in which paraformaldehyde is dissolved, heat to 38° C. under stirring, continue stirring for 0.8 h until the paraformaldehyde is completely dissolved, and then respectively pass through Heaters 5 and 6 are used to preheat the materials to keep isobutylene and formaldehyde hemiacetal fed into the tubular reactor 8 at a molar ratio of 6:1, and the feed space velocity is maintained for 1h -1 , maintain the reaction temperature at 180-190°C, the reaction pressure at 8-9MPa, and continue the reaction for 14 hours. Then the material enters the isobutene recovery tower 10, and the separated isobutene is cooled at -10--15°C and recovered to the isobutene storage tank. Light tower 11, methanol is separated for recycling, the bottom material flows into the product refin...

Embodiment 3

[0036] use figure 1 The shown continuous reaction device carries out the following operation process. Add 80 kg of paraformaldehyde and 350 L of industrial sodium methoxide solution (2%) to the depolymerization kettle 2 in which paraformaldehyde is dissolved, heat to 42° C. under stirring, continue stirring for 1.2 h until the paraformaldehyde is completely dissolved, and then respectively pass through Heaters 5 and 6 are used to preheat the materials to keep isobutylene and formaldehyde hemiacetal fed into the tubular reactor 8 at a molar ratio of 4:1, and the feed space velocity is maintained for 1.5h -1 , maintain the reaction temperature at 160-170°C, the reaction pressure at 9-11MPa, and continue to react for 18 hours. Then the material enters the isobutene recovery tower 10, and the separated isobutene is recovered to the isobutene storage tank after low-temperature cooling at -10--15°C. Light tower 11, methanol is separated for recycling, the bottom material flows into...

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Abstract

The invention discloses a continuous 3-methyl-3-buten-1-ol production method.The method includes that paraformaldehyde is put in corresponding alcoholic solution with sodium methylate or sodium ethoxide mass concentration being 1-5% to form methanal hemiacetal solution by depolymerization and condensation; isobutene and methanal hemiacetal are put in a tubular reactor to generate the target product 3-methyl-3-buten-1-ol by one-step reaction under the action of catalysts; the product generated in the reaction stage is cooled and then fed into an isobutene recovery tower, a light component removal tower and a product refining tower sequentially.By the continuous 3-methyl-3-buten-1-ol production method, the defects of low heat and mass transfer efficiency, high reaction pressure, more side reactions, low production efficiency and the like in an intermittent tank process are overcome, and continuous 3-methyl-3-buten-1-ol production with the isobutene and the methanal hemiacetal serving as raw materials is realized.

Description

technical field [0001] The invention relates to a continuous preparation method of 3-methyl-3-buten-1-ol, a key synthetic raw material of the third-generation polycarboxylic acid high-efficiency water reducer for concrete, and belongs to the technical field of organic chemical industry. Background technique [0002] 3-Methyl-3-butene-1-ol (MBOH) is the initiator of the side chain-TPEG polyether of the third generation polycarboxylate high-efficiency water reducer for synthetic concrete. The TPEG polyether synthesized from this raw material is suitable for The quality and performance of polycarboxylate high-efficiency superplasticizer products play a decisive role, making it have strong ability to maintain the dispersion of cement particles, low dosage, high water-reducing rate, good reinforcement effect, durability, no corrosion of steel bars and Environmentally friendly and other advantages. In addition, 3-methyl-3-buten-1-ol can be isomerized into isopentenol, which is us...

Claims

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Application Information

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IPC IPC(8): C07C33/025C07C29/32
CPCC07C29/32C07C41/56C07C43/30C07C33/025
Inventor 冉千平王涛范士敏杨勇亓帅乔敏马建峰宋峰岩
Owner JIANGSU SOBUTE NEW MATERIALS
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