Poly-conjugate and preparation method thereof

By using di-tert-butyl peroxide in polyclonal synthesis and controlling the reaction temperature and drop acceleration, the safety hazards and finished product quality problems caused by high-active initiators were solved, and a high molecular weight, non-variant color was obtained. , suitable for flame retardant and catalyst, suitable for industrial production.

CN119191928AActive Publication Date: 2024-12-27浙江材华科技有限公司
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Patent Information

Application Number
CN202411699502.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-26
Publication Date
2024-12-27
Estimated Expiration
2044-11-26

AI Technical Summary

Technical Problem

The use of highly active peroxide initiators in the existing polymerization synthesis methods leads to problems such as lower reaction temperature, residual by-products, high safety hazards, yellowish color of finished products, heavy odor and poor mechanical properties.

Method used

Di-tert-butyl peroxide is used as a radical initiator. By controlling the reaction temperature of 130℃~135℃ and drop acceleration, high-active initiators are avoided, and stable synthesis of polyclonal chlorhexidine is achieved, and a white solid product is precipitated.

Benefits of technology

The high molecular weight synthesis of the copolymerized dryness is achieved, the product has no variegated color and no odor, and is in good condition. It is suitable for cross-linked copolymerization catalysts and flame retardant synergistic agents, and is suitable for industrial production.

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Abstract

The invention discloses polymersome and a preparation method thereof, and belongs to the technical field of polymersome synthesis methods. The method comprises the following steps: adding di-tert-butyl peroxide into diisopropylbenzene at the temperature of 130-135 DEG C for reaction, and stopping the reaction until the weight-average molecular weight of a reaction solution obtained by the reaction is not lower than 1850; and precipitating the reaction liquid after the reaction is stopped to obtain solid poly (co-kuhn-co-kuhn). The method is simple to operate, does not use high-activity tert-butyl peroxybenzoate as an initiation accelerator, is low in reaction temperature and free of wastewater and waste materials, and can be used for industrial production. And the prepared poly (coupling agent) finished product is free of mixed color and peculiar smell, good in state and relatively high in molecular weight.
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Description

Technical Field

[0001] The present invention relates to the technical field of poly-anthate synthesis methods, and in particular to a poly-anthate and a preparation method thereof. Background Art

[0002] Diisopropylbenzene oligomer, also known as polyisopropylbenzene, is a oligomer composed of 4 to 7 diisopropylbenzene molecules connected in sequence. The carbon-carbon bond between the quaternary carbon atoms in the polyisopropylbenzene molecule is not very stable and is easily dissociated into free radicals. Based on this characteristic, polyisopropylbenzene is widely used in cross-linking copolymerization catalysts and flame retardant synergists.

[0003] Compared with general free radical small molecule initiators, polyanil has a more stable structure, a more controllable way of generating free radicals, and is safe to use. As a flame retardant synergist, it is widely used in bromine flame retardant systems and can be used to replace antimony trioxide to increase the flame retardant effect. The addition amount of polyanil is generally 2%~3% of the flame retardant masterbatch. It can reduce the amount of flame retardant used during use and increase the mechanical properties of plastics.

[0004] At present, the synthesis method of poly-copper oxide mainly uses peroxide to initiate diisopropylbenzene to form free radicals, and then the free radicals bond with each other to form poly-copper oxide molecules. In general synthesis, in order to increase the molecular weight of poly-copper oxide molecules, a small amount of highly active peroxide with a lower decomposition temperature (the most common one is tert-butyl perbenzoate) is added to increase the selectivity of the reaction. Although the addition of highly active initiators can shorten the reaction time and reduce the reaction temperature, it will also make the poly-copper oxide product yellow and dark, affecting the appearance of the finished product; at the same time, the residual by-products such as benzoic acid generated during the reaction will also make the finished product have a strong odor and become soft and sticky; the stability of benzoyl peroxide is also very poor, which greatly increases the safety risks in the production process.

[0005] In view of this, the present invention is proposed. Summary of the invention

[0006] The object of the present invention is to provide a polyunsaturated polyol and a preparation method thereof to solve or improve the above-mentioned technical problems.

[0007] The present invention can be implemented like this: In a first aspect, the present invention provides a method for preparing poly-copper nitrate, which comprises the following steps: adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. to react until the weight average molecular weight of the reaction solution obtained by the reaction is not less than 1850, and then stopping the reaction; precipitating the reaction solution after the reaction is stopped to obtain a solid poly-copper nitrate.

[0008] In an optional embodiment, diisopropylbenzene is heated to 130° C. to 135° C. in an oil bath.

[0009] In an optional embodiment, the reaction of adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. includes: firstly adding di-tert-butyl peroxide to the diisopropylbenzene at a rate of 1 s / drop to 2 s / drop, and when distillate begins to distill, adjusting the dropping rate of di-tert-butyl peroxide and the oil bath temperature of diisopropylbenzene to control the distillation rate of the distillate to 10 s / drop to 20 s / drop.

[0010] In an alternative embodiment, the actual reaction temperature of the reaction process does not exceed 125°C.

[0011] In an optional embodiment, after the addition of di-tert-butyl peroxide is completed, the reaction temperature is controlled to be 118° C. to 123° C.

[0012] In an optional embodiment, the molar ratio of diisopropylbenzene to di-tert-butyl peroxide is 1:1 to 1:2.

[0013] In an alternative embodiment, the precipitating agent used for precipitation includes at least one of ethanol and methanol.

[0014] In a second aspect, the present invention provides a poly-copolymer prepared by the preparation method of any one of the aforementioned embodiments; The number average molecular weight of the polyoxocyanate is not less than 850; The weight average molecular weight of the polyol is not less than 1850; The melting range of polyunsaturated carbon is 53℃~205℃; Polyoxazine is a white solid powder.

[0015] The beneficial effects of the present invention include: The invention provides a novel preparation method of poly-copolymer, which is simple to operate, does not use highly active tert-butyl peroxybenzoate as an initiator, has a low reaction temperature, a high yield, no wastewater or waste, and can be used for industrial production. The prepared poly-copolymer finished product has no variegated color, no odor, is in good condition, has a high molecular weight, and can be used to further prepare a cross-linked copolymerization catalyst or a flame retardant synergist. DETAILED DESCRIPTION

[0016] In order to make the purpose, technical scheme and advantages of the embodiments of the present invention clearer, the technical scheme in the embodiments of the present invention will be described clearly and completely below. If the specific conditions are not specified in the embodiments, they are carried out according to conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not specified, they are all conventional products that can be purchased commercially.

[0017] The polyol provided by the present invention and its preparation method are described in detail below.

[0018] The invention provides a method for preparing poly-copper nitrate, which comprises the following steps: adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. to react until the weight average molecular weight of the reaction liquid obtained by the reaction is not less than 1850, and then stopping the reaction; and precipitating the reaction liquid after the reaction is stopped to obtain solid poly-copper nitrate.

[0019] The reaction principle is: di-tert-butyl peroxide acts as a free radical initiator, which decomposes into tert-butyl radicals when heated; the tert-butyl radicals will attack diisopropylbenzene, seize the hydrogen of diisopropylbenzene, and turn diisopropylbenzene into diisopropylbenzene radicals. The diisopropylbenzene radicals bond with each other to form oligomer molecules with a degree of polymerization of 7 to 10, namely, polyisopropylbenzene.

[0020] In the present invention, the molar ratio of diisopropylbenzene to di-tert-butyl peroxide can be 1:1 to 1:2, such as 1:1, 1:1.5 or 1:2, or other values ​​within the range of 1:1 to 1:2.

[0021] In some embodiments, before adding di-tert-butyl peroxide, diisopropylbenzene may be heated to 130° C. to 135° C. to remove water.

[0022] The water removal time can be 2 hours by way of example but not limitation.

[0023] By removing water from diisopropylbenzene, it is possible to prevent water from affecting the decomposition of di-tert-butyl peroxide free radicals.

[0024] In some embodiments, diisopropylbenzene may be heated to 130° C. to 135° C. in an oil bath. Specifically, the oil bath temperature of diisopropylbenzene may be 130° C., 131° C., 132° C., 133° C., 134° C., or 135° C., or other values ​​within the range of 130° C. to 135° C.

[0025] In some preferred embodiments, the reaction of adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. comprises: firstly adding di-tert-butyl peroxide to diisopropylbenzene at a rate of 1 s / drop to 2 s / drop (such as 1 s / drop, 1.5 s / drop or 2 s / drop, etc.), and when distillate begins to be distilled out, adjusting the dropping rate of di-tert-butyl peroxide and the oil bath temperature of diisopropylbenzene to control the distillation rate of the distillate to 10 s / drop to 20 s / drop (such as 10 s / drop, 12 s / drop, 14 s / drop, 16 s / drop, 18 s / drop or 20 s / drop, etc.).

[0026] The above diisopropylbenzene is in a stirring state.

[0027] By controlling the order of adding di-tert-butyl peroxide in stages, it is possible to ensure a moderate reaction rate while avoiding the waste of raw materials. If the di-tert-butyl peroxide is added too quickly, the temperature of the reaction system will drop rapidly, and the reaction rate will decrease; at the same time, a large amount of di-tert-butyl peroxide will accumulate in the reaction vessel, which will cause the risk of explosion and pose a great safety hazard. If the di-tert-butyl peroxide is added too slowly, the temperature in the reaction vessel will be too high, so that a large amount of di-tert-butyl peroxide will not participate in the reaction and will be evaporated, resulting in a waste of raw materials.

[0028] In the present invention, the actual reaction temperature of the reaction of diisopropylbenzene and di-tert-butyl peroxide does not exceed 125° C. In some preferred embodiments, after the addition of di-tert-butyl peroxide is completed, the reaction temperature is controlled to be 118° C. to 123° C., such as 118° C., 119° C., 120° C., 121° C., 122° C. or 123° C., or any other value within the range of 118° C. to 123° C.

[0029] The reaction time can be, for example, 15 h to 22 h, such as 15 h, 16 h, 17 h, 18 h, 19 h, 20 h, 21 h or 22 h, etc., depending on the actual situation.

[0030] The reaction can be stopped when the weight average molecular weight of the reaction liquid obtained by the reaction is not less than 1850. The reaction liquid under this condition is viscous like honey, and the mass fraction of di-tert-butyl peroxide in the distillate is less than 1 / 3. If the viscosity of the reaction liquid is low, and the weight average molecular weight of the reaction liquid is less than 1850, or the content of di-tert-butyl peroxide in the distillate exceeds one-third, di-tert-butyl peroxide can be added to continue the reaction until the weight average molecular weight of the reaction liquid is not less than 1850.

[0031] After the reaction stops, the reaction solution can be poured into a precipitant while hot to precipitate to obtain white solid particles, which are then filtered and dried at room temperature to obtain a poly-linked dry product.

[0032] Alternatively, the precipitant may illustratively but not limitatively include at least one of ethanol and methanol.

[0033] In some preferred embodiments, the yield of the preparation method of poly-hydroxybenzene provided by the present invention is not less than 90%.

[0034] As mentioned above, the preparation method of the poly-bis(methoxy)acrylic acid provided by the present invention is simple to operate, and does not use highly active tert-butyl perbenzoate as an initiator promoter. Instead, the stable growth of the molecular weight of the poly-bis(methoxy)acrylic acid is achieved by precisely controlling the material dropwise addition rate and temperature during the reaction process. The process has a low reaction temperature, a high yield, and no wastewater or waste, and can be used for industrial production.

[0035] Correspondingly, the present invention also provides a poly-hydroxybenzoic acid, which is prepared by the above preparation method.

[0036] The finished product of the polyanil has a high molecular weight, is white, not yellow or dark, and has no variegated color; the polyanil has no odor, is solid, is in good condition, and does not become soft or sticky.

[0037] In some embodiments, the number average molecular weight of the polyol provided by the present invention is not less than 850, such as 810, 890, 940, 1100 or 1610.

[0038] In some embodiments, the weight average molecular weight of the polyol provided by the present invention is not less than 1850, such as 1850, 2070, 2100, 3200 or 4540.

[0039] In some embodiments, the melting range of the polyunsaturated copolymer provided by the present invention can be 53°C~205°C, such as 53.7°C~196.0°C, 57.8°C~199.6°C, 60.1°C~201.1°C, 61.1°C~188.2°C or 70.4°C~204.0°C, etc.

[0040] In addition, the present invention also provides an application of the above-mentioned poly-copolymer, for example, the poly-copolymer can be used to prepare a cross-linking copolymer catalyst or a flame retardant synergist.

[0041] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.

[0042] Example 1 This embodiment provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 81.2 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on the mechanical stirring, set the oil bath temperature to 133°C, and remove water for 2 hours.

[0043] S2: After the water is removed, di-tert-butyl peroxide is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of about 1 s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 10 s / drop, and the actual reaction liquid temperature is 123°C.

[0044] S3: After all the di-tert-butyl peroxide (the molar ratio of diisopropylbenzene to di-tert-butyl peroxide is 1:2) has been dripped, the internal temperature is controlled at 123°C to keep the reaction, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0045] S4: After 15 hours of reaction, the reaction liquid is viscous like honey, and the weight average molecular weight of the reaction liquid is 2070, and the reaction is stopped. The reaction liquid is poured into ethanol while hot to precipitate, and white solid particles are obtained. The solid particles are filtered and dried at room temperature to obtain the poly-linked product.

[0046] Example 2 This embodiment provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 81.7 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on the mechanical stirring, set the oil bath temperature to 134°C, and remove water for 2 hours.

[0047] S2: After the water is removed, di-tert-butyl peroxide is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of about 1 s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 10 s / drop, and the actual reaction liquid temperature is 121°C.

[0048] S3: After all the di-tert-butyl peroxide (the molar ratio of diisopropylbenzene to di-tert-butyl peroxide is 1:1.5) has been dripped, the internal temperature is controlled at 121°C to keep the reaction going, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0049] S4: After 21 hours of reaction, the reaction liquid is viscous like honey, and the weight average molecular weight of the reaction liquid is 3200, so the reaction is stopped. The reaction liquid is poured into ethanol while hot to precipitate, and white solid particles are obtained. The particles are filtered and dried at room temperature to obtain the poly-linked product.

[0050] Example 3 This embodiment provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 83.7 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on the mechanical stirring, set the oil bath temperature to 131°C, and remove water for 2 hours.

[0051] S2: After the water is removed, di-tert-butyl peroxide is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of about 1 s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 10 s / drop, and the actual reaction liquid temperature is 121°C.

[0052] S3: After all the di-tert-butyl peroxide (the molar ratio of diisopropylbenzene to di-tert-butyl peroxide is 1:1.8) has been dripped, the internal temperature is controlled at 119°C to keep the reaction, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0053] S4: After 21 hours of reaction, the reaction liquid is viscous like honey, and the weight average molecular weight of the reaction liquid is 1850, so the reaction is stopped. The reaction liquid is poured into ethanol while hot to precipitate, and white solid particles are obtained. The particles are filtered and dried at room temperature to obtain the poly-linked product.

[0054] Example 4 This embodiment provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 80.6 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on the mechanical stirring, set the oil bath temperature to 132°C, and remove water for 2 hours.

[0055] S2: After the water is removed, di-tert-butyl peroxide is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of about 2s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 15s / drop, and the actual reaction liquid temperature is 124°C.

[0056] S3: After all the di-tert-butyl peroxide (the molar ratio of diisopropylbenzene to di-tert-butyl peroxide is 1:1.3) has been dripped, the internal temperature is controlled at 121°C to keep the reaction going, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0057] S4: After 19 hours of reaction, the reaction liquid is viscous like honey, and the weight average molecular weight of the reaction liquid is 2100, so the reaction is stopped. The reaction liquid is poured into ethanol while hot to precipitate, and white solid particles are obtained. The particles are filtered and dried at room temperature to obtain the poly-linked product.

[0058] Example 5 This embodiment provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 83.2 g of diisopropylbenzene into the reaction bottle, insert a thermometer, start mechanical stirring, set the oil bath temperature to 134°C, and remove water for 2 hours.

[0059] S2: After the water is removed, di-tert-butyl peroxide is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of about 2s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 16s / drop, and the actual reaction liquid temperature is 125°C.

[0060] S3: After all the di-tert-butyl peroxide (the molar ratio of diisopropylbenzene to di-tert-butyl peroxide is 1:1.7) has been dripped, the internal temperature is controlled at 119°C to keep the reaction, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0061] S4: After 19 hours of reaction, the reaction liquid is viscous like honey, and the weight average molecular weight of the reaction liquid is 4540, so the reaction is stopped. The reaction liquid is poured into ethanol while hot to precipitate, and white solid particles are obtained. The particles are filtered and dried at room temperature to obtain the poly-linked product.

[0062] Comparative Example 1 This comparative example provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 85.1 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on mechanical stirring, set the oil bath temperature to 133°C, and remove water for 2 hours.

[0063] S2: After the water removal is completed, a peroxide mixture consisting of di-tert-butyl peroxide and tert-butyl perbenzoate (the amount of tert-butyl perbenzoate in the peroxide mixture is 38.9wt%) is slowly added dropwise using a constant pressure dropping funnel, with a dropping speed of about 2s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 15s / drop, and the actual reaction liquid temperature is 125°C.

[0064] S3: After the peroxide mixture (the molar ratio of diisopropylbenzene to the peroxide mixture is 1:1.5) is completely dropped, the internal temperature is controlled at 119°C to keep the reaction, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0065] S4: After 15 hours of reaction, the weight average molecular weight of the reaction solution is 2670, and the reaction is stopped. The reaction solution is poured into ethanol while hot to precipitate, and yellow solid particles with a benzoic acid odor are obtained. The solid particles are filtered and dried at room temperature to obtain the poly-linked product.

[0066] Comparative Example 2 This comparative example provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 83.7 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on the mechanical stirring, set the oil bath temperature to 135°C, and remove water for 2 hours.

[0067] S2: After the water removal is completed, a peroxide mixture consisting of di-tert-butyl peroxide and tert-butyl perbenzoate (the amount of tert-butyl perbenzoate in the peroxide mixture is 19.9wt%) is slowly added dropwise using a constant pressure dropping funnel, with a dropping speed of about 2s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 12s / drop, and the actual reaction liquid temperature is 124°C.

[0068] S3: After the peroxide mixture (the molar ratio of diisopropylbenzene to the peroxide mixture is 1:1.8) is completely dropped, the internal temperature is controlled at 120°C for heat preservation and reaction, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0069] S4: After 17 hours of reaction, the weight average molecular weight of the reaction solution is 980, and the reaction is stopped. The reaction solution is poured into ethanol while hot to precipitate, and yellow waxy solid particles with a benzoic acid odor are obtained. The solid particles are filtered and dried at room temperature to obtain the poly-linked product.

[0070] Comparative Example 3 This comparative example provides a method for preparing poly-linked carbonyl, comprising the following steps: S1: Add 81.0 g of diisopropylbenzene into the reaction bottle, insert a thermometer, turn on the mechanical stirring, set the oil bath temperature to 133°C, and remove water for 2 hours.

[0071] S2: After the water removal is completed, a peroxide mixture consisting of di-tert-butyl peroxide and tert-butyl perbenzoate (the amount of tert-butyl perbenzoate in the peroxide mixture is 30.3wt%) is slowly added dropwise using a constant pressure dropping funnel, with a dropping speed of about 1s / drop. When distillate begins to be distilled out, the oil bath temperature and the dropping speed are controlled so that the distillate distillation speed is 13s / drop, and the actual reaction liquid temperature is 123°C.

[0072] S3: After the peroxide mixture (the molar ratio of diisopropylbenzene to the peroxide mixture is 1:2) is completely dropped, the internal temperature is controlled at 123°C to keep the reaction, and samples are taken every 2 hours to monitor the reaction progress by gas chromatography and GPC.

[0073] S4: After 20 hours of reaction, the weight average molecular weight of the reaction solution is 1160, and the reaction is stopped. The reaction solution is poured into ethanol while hot to precipitate, and yellow waxy solid particles with a benzoic acid odor are obtained. The particles are filtered and dried at room temperature to obtain the poly-linked product.

[0074] Comparative Example 4 The difference between this comparative example and Example 1 is that in S2, when the distillate begins to be distilled out, the distillation rate of the distillate is controlled to be 5 s / drop by adjusting the dropping speed of di-tert-butyl peroxide and the oil bath temperature of diisopropylbenzene.

[0075] Comparative Example 5 The difference between this comparative example and Example 1 is that in S2, when the distillate begins to be distilled out, the distillation rate of the distillate is controlled to be 25 s / drop by adjusting the dropping speed of di-tert-butyl peroxide and the oil bath temperature of diisopropylbenzene.

[0076] Comparative Example 6 The difference between this comparative example and Example 1 is that in S2, the actual reaction temperature of the reaction process is 130°C.

[0077] Comparative Example 7 The difference between this comparative example and Example 1 is that in S3, the internal temperature is controlled at 127°C for heat preservation reaction.

[0078] Comparative Example 8 The difference between this comparative example and Example 1 is that in S4, the reaction time is 10 h.

[0079] Test example Examples 1 to 5 and Comparative Examples 1 to 8 were repeated 3 times respectively, and the dead branches prepared by Examples 1 to 5 and Comparative Examples 1 to 8 were compared. The results are shown in Table 1. The data in Table 1 are the average results of 3 times.

[0080] Table 1 Comparison results

[0081] It can be seen from Table 1 that the poly-anhydride prepared in the embodiment of the present invention can have a better color and product state and a higher yield than the poly-anhydride prepared in Comparative Examples 1 to 8.

[0082] In summary, the present invention avoids the waste of raw materials caused by excessive di-tert-butyl peroxide distilling out when reacting above the boiling point by strictly controlling the reaction temperature and the dripping speed during the reaction without adding an initiator promoter. The method has a high reaction conversion rate and a yield of more than 90%. Compared with the reaction of adding a reaction selective promoter tert-butyl peroxybenzoate, the product color is clean, without variegated color, no odor, and in good condition.

[0083] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for preparing poly-linked carbonyl, characterized in that: The following steps are involved: Adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. to react until the weight average molecular weight of the reaction solution obtained by the reaction is not less than 1850, and then stopping the reaction; precipitating the reaction solution after the reaction is stopped to obtain a solid polyol; The reaction of adding di-tert-butyl peroxide to diisopropylbenzene at a temperature of 130° C. to 135° C. comprises: firstly dropping the di-tert-butyl peroxide into the diisopropylbenzene at a speed of 1 s / drop to 2 s / drop, and when distillate begins to be distilled out, adjusting the dropping speed of the di-tert-butyl peroxide and the oil bath temperature of the diisopropylbenzene to control the distillate distillation speed to be 10 s / drop to 20 s / drop; The actual reaction temperature of the reaction process does not exceed 125°C; After the addition of di-tert-butyl peroxide is completed, the reaction temperature is controlled at 118°C~123°C.

2. The preparation method according to claim 1, characterized in that: Diisopropylbenzene was heated to 130°C~135°C in an oil bath.

3. The preparation method according to claim 1 or 2, characterized in that: The molar ratio of the diisopropylbenzene to the di-tert-butyl peroxide is 1:1 to 1:

2.

4. The preparation method according to claim 1, characterized in that: The precipitating agent used for precipitation includes at least one of ethanol and methanol.

5. A polylinker, characterized in that: Prepared by the preparation method according to any one of claims 1 to 4; The number average molecular weight of the polyoxocyanate is not less than 850; The weight average molecular weight of the polyol is not less than 1850; The melting range of the polyol is 53°C to 205°C; The polyoxazine is a white solid powder.

Citation Information

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