Molecular weight controllable thermal polymerization resin and preparation method thereof

Abstract

The invention belongs to the technical field of thermal polymerization resins, and discloses a molecular weight controllable thermal polymerization resin and a preparation method thereof, the preparation method comprises the following steps: 1, rectification cutting: feeding cracked C9 into a rectification tower, and cutting into light C9, bicyclic enriched liquid and heavy C9 through a rectification process; 2, carrying out thermal polymerization and flash evaporation on the bicyclic enrichment liquid; 3, heavy C9 thermal polymerization and flash evaporation: mixing the heavy C9 with the heavy C9-removed raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and derivatives thereof; step 4, feeding the mixture obtained in the step 4 into another thermal polymerization reactor, and carrying out thermal polymerization reaction; after the reaction is completed, unreacted volatile components are removed through a flash evaporation process, and deep-color thermal polymerization petroleum resin is obtained; step 5, molecular weight control; step 6, performing subsequent treatment; according to the invention, by adjusting the ratio of the reaction materials, the molecular weight of the C9 thermal polymerization resin is accurately regulated and controlled, and the requirements of different fields on the performance of the thermal polymerization resin are met; environmental protection and sustainability are realized.

Description

Technical Field

[0001] The invention belongs to the technical field of thermopolymer resins, and in particular relates to a molecular weight controllable thermopolymer resin and a preparation method thereof. Background Art

[0002] Thermal polymer resins, especially C9 thermal polymer petroleum resins, as an important chemical raw material, are widely used in adhesives, coatings, inks, rubber plasticizers and other fields. The traditional preparation process of C9 thermal polymer petroleum resins often has problems such as uneven molecular weight distribution, unstable product quality, and different color depths. This is mainly due to the complex composition of raw materials and the difficulty in accurately controlling the reaction conditions. In addition, the market has diverse demands for thermal polymer resins with different molecular weight ranges, and traditional preparation methods have limitations in molecular weight regulation, making it difficult to meet customers' customized requirements, especially for the precise regulation of molecular weight: how to adjust the ratio of the reaction materials to achieve precise regulation of the molecular weight of C9 thermal polymer resins to meet the application needs of different fields, thereby improving product quality and stability. Summary of the invention

[0003] In view of the above situation, in order to overcome the defects of the prior art, the present invention provides a molecular weight controllable thermopolymer resin and a preparation method thereof, which effectively solves the limitations of traditional preparation methods in molecular weight regulation and is difficult to meet customers' customized requirements, especially for the precise control of molecular weight: how to achieve precise control of the molecular weight of C9 thermopolymer resin by adjusting the ratio of reaction materials to meet the application requirements of different fields, thereby improving product quality and stability.

[0004] To achieve the above object, the present invention provides the following technical solution: a method for preparing a molecular weight controllable thermopolymer resin, comprising the following steps:

[0005] Step 1, distillation and cutting:

[0006] The cracked carbon nine is sent to a distillation tower and cut into light carbon nine, double-ring enriched liquid and heavy carbon nine through a distillation process;

[0007] Step 2: Thermal polymerization and flash evaporation of the double-ring enriched liquid:

[0008] The dicyclopentadiene enriched liquid is mixed with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives; the mixture is sent to a thermal polymerization reactor to carry out a thermal polymerization reaction, and after the reaction is completed, the unreacted volatile matter is removed by a flash evaporation process to obtain a light-colored thermally polymerized petroleum resin;

[0009] Step 3, thermal polymerization and flash evaporation of heavy carbon nine: mixing heavy carbon nine with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives;

[0010] Step 4, sending the mixture of step 4 into another thermal polymerization reactor to carry out thermal polymerization reaction; after the reaction is completed, removing unreacted volatiles through a flash evaporation process to obtain a dark thermal polymerization petroleum resin;

[0011] Step 5, molecular weight control: by adjusting the ratio of the de-weighted C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives in the reaction material, the molecular weight of the C9 thermal polymer resin is regulated;

[0012] Step six, subsequent treatment: filtering and drying the obtained light-colored and dark-colored thermally polymerized petroleum resins to remove impurities and improve product quality.

[0013] The mass ratio of the bicyclo enriched liquid in the step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 50-150:30-70:5-15:3-10:3-5.

[0014] The mass ratio of the bicyclo enriched liquid in the step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 100:60:10:7:4.

[0015] The reaction temperature in the step 2 is between 150° C. and 300° C., the reaction time is between 4 hours and 15 hours, and the pressure during the flash evaporation is between 6 mbar and 40 mbar.

[0016] The mass ratio of heavy carbon nine to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives in the step three is 50-200: 50-250: 3-10: 5-15: 3-7.

[0017] The mass ratio of heavy carbon nine to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives in the step three is 100:150:7:10:6.

[0018] The reaction temperature in step 3 is between 150° C. and 300° C., the reaction time is between 4 hours and 15 hours, and the pressure during the flash evaporation is between 6 mbar and 40 mbar.

[0019] A molecular weight controllable thermopolymer resin and a preparation method thereof are provided, and the resin is prepared by the preparation method of the molecular weight controllable thermopolymer resin.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] The molecular weight of the present invention is precisely regulated: by adjusting the ratio of the reaction materials, the molecular weight of the C9 thermopolymer resin is precisely regulated, and the requirements for the performance of the thermopolymer resin in different fields are met; environmental protection and sustainability: the method of the present invention reduces the generation of waste during the preparation process, which is beneficial to environmental protection and sustainable development; the preparation method of the molecular weight controllable thermopolymer resin provided by the present invention has made significant progress in raw material utilization, reaction condition optimization, molecular weight regulation and product quality improvement, and has broad market application prospects. DETAILED DESCRIPTION

[0022] The technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0023] The present invention relates to a method for preparing a molecular weight controllable thermopolymer resin, comprising the following steps:

[0024] Step 1, distillation and cutting:

[0025] The cracked carbon nine is sent to a distillation tower and cut into light carbon nine, double-ring enriched liquid and heavy carbon nine through a distillation process;

[0026] Step 2: Thermal polymerization and flash evaporation of the double-ring enriched liquid:

[0027] The dicyclopentadiene enriched liquid is mixed with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives; the mixture is sent to a thermal polymerization reactor to carry out a thermal polymerization reaction, and after the reaction is completed, the unreacted volatile matter is removed by a flash evaporation process to obtain a light-colored thermally polymerized petroleum resin;

[0028] Step 3, thermal polymerization and flash evaporation of heavy carbon nine: mixing heavy carbon nine with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives;

[0029] Step 4, sending the mixture of step 4 into another thermal polymerization reactor to carry out thermal polymerization reaction; after the reaction is completed, removing unreacted volatiles through a flash evaporation process to obtain a dark thermal polymerization petroleum resin;

[0030] Step 5, molecular weight control: by adjusting the ratio of the de-weighted C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives in the reaction material, the molecular weight of the C9 thermal polymer resin is regulated;

[0031] Step six, subsequent treatment: filtering and drying the obtained light-colored and dark-colored thermally polymerized petroleum resins to remove impurities and improve product quality.

[0032] The mass ratio of the bicyclo enriched liquid in step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 50-150:30-70:5-15:3-10:3-5.

[0033] The mass ratio of the bicyclo enriched liquid in step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 100:60:10:7:4.

[0034] The reaction temperature in step 2 is between 150° C. and 300° C., the reaction time is between 4 hours and 15 hours, and the pressure during the flash evaporation is between 6 mbar and 40 mbar.

[0035] The mass ratio of heavy carbon nine in step three to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives is 50-200:50-250:3-10:5-15:3-7.

[0036] The mass ratio of heavy carbon nine in step three to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives is 100:150:7:10:6.

[0037] The reaction temperature in step 3 is between 150° C. and 300° C., the reaction time is between 4 hours and 15 hours, and the pressure during the flash evaporation is between 6 mbar and 40 mbar.

[0038] A molecular weight controllable thermopolymer resin and a preparation method thereof are prepared by a molecular weight controllable thermopolymer resin preparation method.

[0039] Embodiment 1:

[0040] This embodiment relates to a method for preparing a molecular weight controllable thermopolymer resin, comprising the following steps:

[0041] Step 1, distillation and cutting:

[0042] The cracked carbon nine is sent to a distillation tower and cut into light carbon nine, double-ring enriched liquid and heavy carbon nine through a distillation process;

[0043] Step 2: Thermal polymerization and flash evaporation of the double-ring enriched liquid:

[0044] The dicyclopentadiene enriched liquid is mixed with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives; the mixture is sent to a thermal polymerization reactor to carry out a thermal polymerization reaction, and after the reaction is completed, the unreacted volatile matter is removed by a flash evaporation process to obtain a light-colored thermally polymerized petroleum resin;

[0045] Step 3, thermal polymerization and flash evaporation of heavy carbon nine: mixing heavy carbon nine with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives;

[0046] Step 4, sending the mixture of step 4 into another thermal polymerization reactor to carry out thermal polymerization reaction; after the reaction is completed, removing unreacted volatiles through a flash evaporation process to obtain a dark thermal polymerization petroleum resin;

[0047] Step 5, molecular weight control: by adjusting the ratio of the de-weighted C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives in the reaction material, the molecular weight of the C9 thermal polymer resin is regulated;

[0048] Step six, subsequent treatment: filtering and drying the obtained light-colored and dark-colored thermally polymerized petroleum resins to remove impurities and improve product quality.

[0049] The mass ratio of the bicyclo enriched liquid in step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 50:30:5:3:3.

[0050] The reaction temperature in step 2 is 150° C., the reaction time is 15 hours, and the pressure during the flash evaporation is between 40 mbar.

[0051] The mass ratio of heavy carbon nine in step three to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives is 50:50:3:5:3.

[0052] The reaction temperature in step 3 is 150° C., the reaction time is 15 hours, and the pressure during the flash evaporation is between 40 mbar.

[0053] After testing the obtained products, they pass the testing indicators.

[0054] Embodiment 2:

[0055] This embodiment relates to a method for preparing a molecular weight controllable thermopolymer resin, comprising the following steps:

[0056] Step 1, distillation and cutting:

[0057] The cracked carbon nine is sent to a distillation tower and cut into light carbon nine, double-ring enriched liquid and heavy carbon nine through a distillation process;

[0058] Step 2: Thermal polymerization and flash evaporation of the double-ring enriched liquid:

[0059] The dicyclopentadiene enriched liquid is mixed with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives; the mixture is sent to a thermal polymerization reactor to carry out a thermal polymerization reaction, and after the reaction is completed, the unreacted volatile matter is removed by a flash evaporation process to obtain a light-colored thermally polymerized petroleum resin;

[0060] Step 3, thermal polymerization and flash evaporation of heavy carbon nine: mixing heavy carbon nine with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives;

[0061] Step 4, sending the mixture of step 4 into another thermal polymerization reactor to carry out thermal polymerization reaction; after the reaction is completed, removing unreacted volatiles through a flash evaporation process to obtain a dark thermal polymerization petroleum resin;

[0062] Step 5, molecular weight control: by adjusting the ratio of the de-weighted C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives in the reaction material, the molecular weight of the C9 thermal polymer resin is regulated;

[0063] Step six, subsequent treatment: filtering and drying the obtained light-colored and dark-colored thermally polymerized petroleum resins to remove impurities and improve product quality.

[0064] The mass ratio of the bicyclo enriched liquid in step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 150:70:15:10:5.

[0065] The reaction temperature in step 2 is 300° C., the reaction time is 15 hours, and the pressure during the flash evaporation is 6 mbar.

[0066] The mass ratio of heavy carbon nine in step three to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives is 200:250:10:15:7.

[0067] The reaction temperature in step 3 is 300° C., the reaction time is 15 hours, and the pressure during the flash evaporation is 6 mbar.

[0068] After testing the obtained products, they pass the testing indicators.

[0069] Embodiment 3:

[0070] This embodiment relates to a method for preparing a molecular weight controllable thermopolymer resin, comprising the following steps:

[0071] Step 1, distillation and cutting:

[0072] The cracked carbon nine is sent to a distillation tower and cut into light carbon nine, double-ring enriched liquid and heavy carbon nine through a distillation process;

[0073] Step 2: Thermal polymerization and flash evaporation of the double-ring enriched liquid:

[0074] The dicyclopentadiene enriched liquid is mixed with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives; the mixture is sent to a thermal polymerization reactor to carry out a thermal polymerization reaction, and after the reaction is completed, the unreacted volatile matter is removed by a flash evaporation process to obtain a light-colored thermally polymerized petroleum resin;

[0075] Step 3, thermal polymerization and flash evaporation of heavy carbon nine: mixing heavy carbon nine with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives;

[0076] Step 4, sending the mixture of step 4 into another thermal polymerization reactor to carry out thermal polymerization reaction; after the reaction is completed, removing unreacted volatiles through a flash evaporation process to obtain a dark thermal polymerization petroleum resin;

[0077] Step 5, molecular weight control: by adjusting the ratio of the de-weighted C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives in the reaction material, the molecular weight of the C9 thermal polymer resin is regulated;

[0078] Step six, subsequent treatment: filtering and drying the obtained light-colored and dark-colored thermally polymerized petroleum resins to remove impurities and improve product quality.

[0079] The mass ratio of the bicyclo enriched liquid in step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 100:60:10:7:4.

[0080] The reaction temperature in step 2 is 200° C., the reaction time is 10 hours, and the pressure during the flash evaporation is 25 mbar.

[0081] The mass ratio of heavy carbon nine in step three to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives is 100:150:7:10:6.

[0082] The reaction temperature in step 3 is 200° C., the reaction time is 10 hours, and the pressure during the flash evaporation is 25 mbar.

[0083] After testing the obtained products, they pass the testing indicators.

[0084] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.

[0085] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a molecular weight controllable thermopolymer resin, characterized in that: The following steps are involved: Step 1, distillation and cutting: The cracked carbon nine is sent to a distillation tower and cut into light carbon nine, double-ring enriched liquid and heavy carbon nine through a distillation process; Step 2: Thermal polymerization and flash evaporation of the double-ring enriched liquid: The dicyclopentadiene enriched liquid is mixed with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives; the mixture is sent to a thermal polymerization reactor to carry out a thermal polymerization reaction, and after the reaction is completed, the unreacted volatile matter is removed by a flash evaporation process to obtain a light-colored thermally polymerized petroleum resin; Step 3, thermal polymerization and flash evaporation of heavy carbon nine: mixing heavy carbon nine with the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives; Step 4, sending the mixture of step 4 into another thermal polymerization reactor to carry out thermal polymerization reaction; after the reaction is completed, removing the unreacted volatile matter through a flash evaporation process to obtain a dark thermal polymerization petroleum resin; Step 5, molecular weight control: by adjusting the ratio of the de-weighted C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives in the reaction material, the molecular weight of the C9 thermal polymer resin is regulated; Step six, subsequent treatment: filtering and drying the obtained light-colored and dark-colored thermally polymerized petroleum resins to remove impurities and improve product quality.

2. The method for preparing a molecular weight controllable thermopolymer resin according to claim 1, characterized in that: The mass ratio of the bicyclo enriched liquid in the step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 50-150:30-70:5-15:3-10:3-5.

3. The method for preparing a molecular weight controllable thermopolymer resin according to claim 2, characterized in that: The mass ratio of the bicyclo enriched liquid in the step 2 to an appropriate amount of the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene and styrene and its derivatives is 100:60:10:7:

4.

4. The method for preparing a molecular weight controllable thermopolymer resin according to claim 1, characterized in that: The reaction temperature in the step 2 is between 150° C. and 300° C., the reaction time is between 4 hours and 15 hours, and the pressure during the flash evaporation is between 6 mbar and 40 mbar.

5. The method for preparing a molecular weight controllable thermopolymer resin according to claim 1, characterized in that: The mass ratio of heavy carbon nine to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives in the step three is 50-200: 50-250: 3-10: 5-15: 3-7.

6. The method for preparing a molecular weight controllable thermopolymer resin according to claim 5, characterized in that: The mass ratio of heavy carbon nine to the de-heavy C9 raw material, dicyclopentadiene, methyl dicyclopentadiene, styrene and its derivatives in the step three is 100:150:7:10:

6.

7. The method for preparing a molecular weight controllable thermopolymer resin according to claim 1, characterized in that: The reaction temperature in step 3 is between 150° C. and 300° C., the reaction time is between 4 hours and 15 hours, and the pressure during the flash evaporation is between 6 mbar and 40 mbar.

8. A molecular weight controllable thermopolymer resin and a preparation method thereof, characterized in that: The invention is prepared by the method for preparing a molecular weight controllable thermopolymer resin according to any one of claims 1 to 7.