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Purification process of octamethylcyclotetrasiloxane

An octamethylcyclotetrasiloxane and process technology, applied in the direction of silicon organic compounds, etc., can solve problems such as complex operation process, achieve the effects of high process integration, low metal impurity content, and saving operating costs

Pending Publication Date: 2020-08-25
GRINM GUOJINGHUI NEW MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the patent CN108929343A, low-temperature crystallization coupled rectification of solvent is used to purify D4. Although this process can effectively remove the high and low boiling points in D4, it is harmful to the H in the product. 2 O and O 2 There is no effective control, and the operation process is relatively complicated

Method used

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  • Purification process of octamethylcyclotetrasiloxane

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Experimental program
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Effect test

Embodiment 1 8

[0029] The purification process X1 of embodiment 1 octamethylcyclotetrasiloxane

[0030] Such as figure 1 As shown, the industrial octamethylcyclotetrasiloxane (D4) with a content of 90% and the adsorbent PEI / SiO 2 According to the ratio of 1:0.01 into the reactive distillation column. Introduce high-purity argon, start the pneumatic agitator, and heat the tower kettle to 168-178°C under negative pressure of -1 to -3k Pa. After maintaining the slight boiling state for 2 hours, increase the heating power, and react with total reflux for 3 hours, and control the reflux Ratio 4:1~12:1, cut off the fraction between 170~180°C to obtain the D4 intermediate product of primary rectification; combine the high boiling point residual liquid with PEI / SiO 2 released from the bottom of the tower.

[0031] The primary rectification D4 intermediate product obtained by the reactive distillation tower is introduced into the secondary rectification tower along with the pipeline, and the high-...

Embodiment 2 8

[0034] The purification process X2 of embodiment 2 octamethylcyclotetrasiloxane

[0035] Put D4 with a content of 90% and adsorbent 13X molecular sieve into the reactive distillation column according to the ratio of 1:0.005. Introduce high-purity argon, start the air flow agitator, and heat the tower kettle to 168-178°C under negative pressure of -2 to -3k Pa. After maintaining the slight boiling state for 1 hour, increase the heating power, and react with total reflux for 3 hours, and control the reflux The ratio is 4:1~12:1, and the fraction between 170~180°C is cut off to obtain the D4 intermediate product of primary rectification; the high boiling point residual liquid and 13X molecular sieve are released from the bottom of the tower.

[0036] The primary rectification D4 intermediate product obtained by the reactive distillation tower is introduced into the secondary rectification tower along with the pipeline, and the flow rate of the empty tower is 3.0×10 -3 m / s high-p...

Embodiment 3 8

[0039] The purification process X3 of embodiment 3 octamethylcyclotetrasiloxane

[0040] Put the industrial octamethylcyclotetrasiloxane (D4) with a content of 90% and the adsorbent disodium ethylenediamine tetraacetate into the reactive distillation column according to the ratio of 1:0.01. Introduce high-purity argon, start the pneumatic agitator, and heat the tower kettle to 168-178°C under negative pressure of -15~-20kPa. After maintaining the slight boiling state for 10 hours, increase the heating power, and perform full reflux reaction for 3 hours, and control the reflux The ratio is 4:1~12:1, and the fraction between 170~180°C is intercepted to obtain the D4 intermediate product of primary rectification; the high boiling point residual liquid and disodium ethylenediaminetetraacetic acid are released from the bottom of the tower.

[0041] The initial rectification D4 intermediate product obtained by the reactive distillation tower is introduced into the secondary rectific...

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Abstract

The invention relates to a purification process of octamethylcyclotetrasiloxane. The purification process comprises the following steps: by using high-purity argon as a carrier gas, removing metal impurities in octamethylcyclotetrasiloxane by an adsorption reaction in a slight boiling state; carrying out rectification purification, separating octamethylcyclotetrasiloxane from the adsorbent, and removing organic impurities, water and oxygen to obtain an octamethylcyclotetrasiloxane intermediate product; and conducting secondary rectification to further purify an octamethylcyclotetrasiloxane intermediate product so as to obtain a pure octamethylcyclotetrasiloxane product with purity of greater than 99.999%. The pure octamethylcyclotetrasiloxane product meets the cladding deposition requirement of an optical fiber preform.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, in particular to a purification process of octamethylcyclotetrasiloxane. Background technique [0002] Since the beginning of large-scale production of optical fibers in the late 1970s, chemical vapor deposition has been widely used in the world to produce optical fiber preforms, and halogen-containing materials such as silicon tetrachloride have always been the first choice for optical fiber manufacturing raw materials. Compared with the traditional silicon tetrachloride material for optical fiber preform deposition, octamethylcyclotetrasiloxane (octamethylcyclotetrasiloxane, D 4 , OMCTS) have attracted the attention of researchers because they are non-toxic, non-corrosive and will not produce toxic and highly corrosive products after pyrolysis. [0003] In order to improve the transmission performance of the optical fiber and reduce the extrinsic absorption loss of t...

Claims

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Application Information

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IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 蒲云平莫杰冯晓青赵强胡通任剑纪淼
Owner GRINM GUOJINGHUI NEW MATERIALS CO LTD
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