Industrial continuous process for preparation of p-tert-butylphenol

A technology of p-tert-butylphenol and phenol, which is applied in the field of preparation of tert-butylphenol and continuous industrialization, can solve the problems of low conversion rate, difficult treatment, difficult product separation, etc., and achieve high conversion rate, good selectivity and high yield high effect

Inactive Publication Date: 2018-09-21
QINGDAO UNIV
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Problems solved by technology

[0003] The industrial synthesis of p-tert-butylphenol mainly uses phenol and isobutylene as raw materials. The catalytic system first used sulfuric acid as a catalyst, and later extended to other protonic acids or Lewis acids, such as phosphoric acid, boron trifluoride, hydrogen fluoride, trichloro Aluminum, etc., but this method has the disadvantages of phenolic water pollution, corrosion equipment, poor product quality, many side reactions, and difficult separation of catalyst and product.
In order to overcome the above shortcomings, the patent US 426083 loads protonic acid or Lewis acid on an inorganic carrier, such as activated clay or acid clay. This method not only improves the utilization rate of isobutene, but also the product does not need to be washed, effectively solving the problem of phenolic water pollution. However, a large amount of catalyst waste residue will be produced during production, which is difficult to handle and is not suitable for large-scale industrial production
Chinese patent CN1572760A introduces a method for synthesizing tert-butylphenol with MTBE as an alkylation reagent. This patent uses a double-tank reactor, which cannot be continuously produced, and MTBE will be used as a by-product of methanol. The methanol generated in the reaction must be gradually removed from the reaction system, otherwise the conversion rate of the reaction is low
Cationic resin is used as the catalyst, the reaction conditions are mild, and there is no corrosion, but there are still problems such as low reaction selectivity, many by-products, and difficult product separation.
[0005] The ratio of isobutene and phenol has a great influence on the composition of the alkylation liquid. Excessive isobutene will lead to a large number of disubstituted products or even multi-substituted products in the final composition of the alkylated liquid. Insufficient isobutene will reduce the conversion rate of phenol , thus seriously affecting the quality of the alkylating liquid, bringing enormous pressure to the separation and purification of the product and the production cost

Method used

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  • Industrial continuous process for preparation of p-tert-butylphenol

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Effect test

Embodiment 1

[0013] Embodiment 1: With phenol and isobutylene as raw materials, under the action of catalyst, the fixed-bed reactor that is continuously operated in series by multiple kettles, the reactor is a fixed-bed reactor operated continuously in series with multiple kettles, and the catalyst filling capacity of the reactor accounts for 50% of the volume, the number of multiple reactors connected in series is 2, phenol is added from the first reactor, isobutene is added continuously through multiple reactors, the ratio of phenol and isobutene in each reactor is 1:0.3, and each reactor The reaction temperature range is: 60°C, the reaction pressure is 0MPa, the quality control rate is: 0.5, the reaction device is directly connected to the rectification device to separate the raw material and the product, the raw material is returned to the catalytic tower to complete the continuous operation, and the product is rectified Connects directly to product tank.

Embodiment 2

[0014] Embodiment 2: With phenol and isobutylene as raw materials, under the action of catalyst, the fixed-bed reactor of multi-still series continuous operation, the reactor is the fixed-bed reactor of multi-still series continuous operation, and the catalyst filling capacity of the reactor accounts for 80% of the volume, the number of multiple reactors connected in series is 4, phenol is added from the first reactor, isobutene is added continuously through multiple reactors, the ratio of phenol and isobutene in each reactor is 1:1, each reactor The reaction temperature range is: 180°C, the reaction pressure is 3.0MPa, and the quality control rate is: 3.0. The reaction device is directly connected to the rectification device to separate the raw material and the product, and the raw material is returned to the catalytic tower to complete the continuous operation. Distillation is connected directly to the product storage tank.

Embodiment 3

[0015] Embodiment 3: With phenol and isobutylene as raw materials, under the action of catalyst, through the fixed-bed reactor of continuous operation of multi-still series, the reactor is a fixed-bed reactor of multi-kettle series continuous operation, and the catalyst filling capacity of reactor accounts for 60% of the volume, the number of multiple reactors connected in series is 6, phenol is added from the first reactor, isobutene is added continuously through multiple reactors, and the ratio of phenol and isobutene in each reactor is 1:0.5, and each reactor The reaction temperature range is: 120°C, the reaction pressure is 2.0MPa, and the quality control rate is: 2.0. The reaction device is directly connected to the rectification device to separate the raw material and the product, and the raw material is returned to the catalytic tower to complete the continuous operation. Distillation is connected directly to the product storage tank.

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Abstract

The invention discloses an industrial continuous process for preparation of p-tert-butylphenol. According to the process, phenol and isobutene are used as raw materials and allowed to pass through a fixed-bed reactor under the action of a catalyst, wherein continuous operation via multiple tandem kettles is carried out in the fixed-bed reactor; phenol is added from a first kettle; isobutene is added in a manner of multi-kettle continuous introduction; a reaction device is directly connected with a rectification device for separation of the raw materials and a product; the raw materials are returned to a catalytic tower for continuous operation; and the product is directly connected with a product storage tank after rectification. The method has the beneficial effects of good selectivity, high conversion rate, high yield, and almost no wastewater during production.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and relates to an industrialized continuous method for preparing tert-butylphenol. Background technique [0002] p-tert-butylphenol is an important raw material of p-tert-phenol formaldehyde resin, widely used in the synthesis of oil-soluble phenolic resin, plasticizer of synthetic rubber, anti-cracking agent, stabilizer of styrene and butadiene, high-grade ink and paint additives, etc. In addition to being a wide range of additives, it is also an intermediate of many high-performance additives used in oil refining, petrochemical and polymer material industries. [0003] The industrial synthesis of p-tert-butylphenol mainly uses phenol and isobutylene as raw materials. The catalytic system first used sulfuric acid as a catalyst, and later extended to other protonic acids or Lewis acids, such as phosphoric acid, boron trifluoride, hydrogen fluoride, trichloro However, this method has di...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/14C07C37/74
CPCC07C37/14C07C37/74C07C39/06Y02P20/52
Inventor 姜鹏方龙陈照军杜辉
Owner QINGDAO UNIV
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