A kind of polycarbonate and its synthesis method, rigid monomer and its preparation method

A technology of polycarbonate and synthesis method, which is applied in the preparation of carboxylic acid esters, carbon-based compounds, hydroxyl compounds, etc., and can solve problems such as poor yellowing resistance, cancer induction, precocious puberty in infants, and lack of weather resistance. , to achieve the effect of good sustainable development, easy structure and function, and low price

Active Publication Date: 2021-08-27
JIANGSU GUOWANG HIGH TECH FIBER CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, BPA is derived from petroleum resources, and BPA is a hormone analogue, which has the risk of inducing cancer and premature puberty in infants. Countries all over the world are banning BPA-PC from being used in food and pharmaceutical packaging, and its yellowing resistance is not good. , especially when it comes to outdoor products, the weather resistance is lacking

Method used

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  • A kind of polycarbonate and its synthesis method, rigid monomer and its preparation method
  • A kind of polycarbonate and its synthesis method, rigid monomer and its preparation method
  • A kind of polycarbonate and its synthesis method, rigid monomer and its preparation method

Examples

Experimental program
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Embodiment 1

[0070] This example provides a preparation method for the compound (2,4,6,8-tetramethylbicyclo[3.3.0]octane-3,7-diol) represented by formula (I), and its synthetic route is as follows, wherein M is sodium:

[0071]

[0072] (1) Under ice bath, add 125 mL of methanol to a 500 mL round-bottomed flask equipped with a magnetic stirrer, slowly add 7.04 g (0.176 mol) of NaOH, and slowly dropwise add 30 g (0.172 mol) of 1.3- Dimethyl acetonedicarboxylate, heated to reflux at 65°C for 4 h, added 5.7 g (0.098 mol) glyoxal, reacted at room temperature for 12 h, filtered with suction, washed with 30 mL of methanol, dried to obtain the compound represented by formula (Ⅴ) , the yield is about 70%.

[0073] (2) Dissolve the compound represented by formula (Ⅴ) obtained in step (1) in distilled water, add hydrochloric acid (1mol / L) to acidify, then extract with ethyl acetate, wash with saturated sodium bicarbonate solution, anhydrous Na 2 SO 4 After drying and spin-drying ethyl acetate,...

Embodiment 2

[0077] This example provides a preparation method of the compound (2,4,6,8-tetramethylbicyclo[3.3.0]octane-3,7-diol) represented by formula (I), which includes the following steps:

[0078] The steps for preparing the compound represented by formula (II) are the same as in Example 1.

[0079] Under ice-bath conditions, add 5.0 g of the compound represented by formula (II) into a round-bottomed flask equipped with a stirring magnet, add 100 mL of anhydrous methanol, 0.10 mol of sodium borohydride, and react at 0°C for 8 h. Continue to react for 4 h. After the reaction, add 50 mL of distilled water, 125 mL (2 M) of hydrochloric acid, extract with 4×50 mL of ethyl acetate, dry over anhydrous magnesium sulfate, filter with suction, and rotary evaporate to obtain the rigid single 2,4,6,8-tetramethylbicyclo[3.3.0]octane-3,7-diol with a yield of 85%.

Embodiment 3

[0081] This example provides a kind of preparation method of homopolycarbonate, and it comprises the steps:

[0082] Add 1.98 g (10 mmol) of 2,4,6,8-tetramethylbicyclo[3.3.0]octane-3,7-diol prepared in Example 1 and 2.14 g (10 mmol) diphenyl carbonate, add catalyst lithium acetylacetonate and 4-dimethylaminopyridine (mass ratio of feed is 1:1, total feed 0.015 g), slowly feed nitrogen and continue stirring, heat to 140 ° C, at this temperature React for 3 h. The nitrogen protection was removed, the vacuum was changed to 0.5 mmHg, the temperature was raised to 200°C, and the reaction was continued for 8 h. The reaction solution was cooled to room temperature, dissolved by adding 2 mL of chloroform, precipitated by cold methanol, and a light yellow solid was precipitated, which was filtered by suction and fully dried to obtain homopolycarbonate.

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Abstract

The invention discloses a polycarbonate and its synthesis method, rigid monomer and its preparation method. The polycarbonate contains the structural unit shown in the following formula (i): (i); The structure shown: the synthesis of the polycarbonate not only makes the synthesized polycarbonate overcome the defects of the existing polycarbonate BPA-PC, but also is biodegradable, easy to realize the diversification of structure and function, good weather resistance, and industrialized Potential, meet environmental protection requirements; especially the rigid monomer of the present invention can be prepared by using bio-based materials such as citric acid, the source of raw materials is wide, low in price, renewable, can reduce dependence on petroleum resources from the source, and is conducive to industrial applications .

Description

technical field [0001] The invention relates to the technical field of renewable resource utilization and green synthesis, in particular to the synthesis of polycarbonate by using renewable resources, in particular to a polycarbonate and a synthesis method thereof, a rigid monomer and a preparation method thereof. Background technique [0002] Polycarbonate is a high molecular polymer containing carbonate bonds in its molecular chain. According to the type of monomer, it can be divided into three types: aliphatic, aromatic and aliphatic-aromatic. Typically, polycarbonate refers to bisphenol A-based polycarbonate (BPA-PC). BPA-PC has high transparency, high refractive index, strong impact resistance and excellent processing performance, and is widely used in many fields such as optics, electronics, automobiles, construction, office equipment, packaging, and medical care. However, BPA is derived from petroleum resources, and BPA is a hormone analogue, which has the risk of in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G64/30C07C35/31C07C29/143C07C67/343C07C69/757C07C67/31C07C45/67C07C49/443
CPCC08G64/305C07C35/31C07C29/143C07C67/343C07C67/31C07C45/676C07C2602/22C07C69/757C07C49/443
Inventor 高国洪庞成才田会双袁俊祥
Owner JIANGSU GUOWANG HIGH TECH FIBER CO LTD
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