A process for the preparation of a beta-pinene liquid resin

Abstract

The application discloses a preparation method of beta-pinene liquid resin, and comprises the following steps: stirring the analytical pure AR toluene in a three-necked reaction bottle at a stirring speed of 500 / min, starting a constant-temperature water bath to reduce the temperature to 30 DEG C, putting 3g of analytical pure AR aluminum chloride into the three-necked reaction bottle at one time, uniformly mixing 92g of beta pinene with a content of 98% and 8g of perfume grade terpineol, and putting the mixture into a 125ml constant-pressure dropping funnel, starting to drop the beta pinene when the temperature in the reaction bottle is reduced to 30 DEG C, stopping dropping when the temperature in the reaction bottle is increased to 55 DEG C, controlling the dropping temperature at 55 DEG C-60 DEG C, until the dropping is completed, at this time, the polymerization liquid turns into wine red, hydrolysis and water washing are carried out after constant temperature is kept to 40 DEG C for 2 hours, then, toluene is removed at 160 DEG C, vacuum is extracted at 225 DEG C to 0.092Mpa, and the material is discharged; the beta-pinene liquid resin prepared by the method has fluidity, high cohesion, high viscosity and high peeling strength.

Description

Technical Field

[0001] This invention specifically relates to a method for preparing β-pinene liquid resin. Background Technology

[0002] β-Pinene is one of the main components of turpentine, a natural chemical produced by processing pine resin through cutting pine trees. Turpentine is a multi-component mixture, with its main components being α-pinene, β-pinene, dipentene, and longifolene. Resins formed by polymerizing turpentine and its monomers using a Lewis acid system as a catalyst are collectively called terpene resins (also known as pinene resins). Based on the product's form, they are further classified into solid terpene (pinene) resins and liquid terpene (pinene) resins. Based on the source and use of raw materials, as well as the application performance requirements of the product, they can also be divided into ordinary terpene (pinene) resins (these products are manufactured using turpentine as the raw material).

[0003] α-pinene resin and β-pinene resin, etc. (These products are produced by distilling turpentine oil to separate α-pinene and β-pinene, which are then used separately). Currently, ordinary production technology can only produce liquid terpene resins using common turpentine oil, α-pinene, and dipentene as raw materials. However, due to its highly reactive and easily polymerized molecular structure, β-pinene can only be used to produce solid terpene resins.

[0004] The raw materials currently used to produce liquid terpene (pinene) resin are mixed compounds mainly composed of α-pinene, dipentene, and longifene. Due to their molecular structure—specifically, the double bonds are within a ring—these compounds are relatively stable. Even under the catalysis of Lewis acids, the double bonds within the ring structure are not easily broken, hindering polymerization. This facilitates the formation of low-molecular-weight trimers and tetramers, resulting in liquid terpene resin as the final product. Currently, liquid terpene resins produced from these raw materials exhibit good initial tack, good flowability, and low viscosity due to the influence of the raw material's molecular structure. However, they also suffer from low cohesive strength, weak peel strength, and relatively low viscosity. Summary of the Invention

[0005] To overcome the shortcomings and disadvantages of the prior art, the primary objective of this invention is to provide a method for preparing β-pinene liquid resin. This method for preparing β-pinene liquid resin has both fluidity and high cohesive strength, as well as high viscosity and peel strength. Furthermore, the polymer products produced from β-pinene due to its molecular structure possess the aforementioned characteristics. Therefore, based on the characteristics of β-pinene resin, it has such advantages.

[0006] The primary objective of this invention is achieved through the following technical solution:

[0007] A method for preparing a β-pinene liquid resin includes the following steps:

[0008] Take a three-necked reaction flask with a capacity of 250 ml, add analytical grade AR toluene to it, the amount of toluene is 100 g ± 10%, and adjust the stirring speed of the reaction flask to 500 r / min ± 10%.

[0009] Analytical grade AR aluminum trichloride was added to the above reaction flask in one go. The amount of aluminum trichloride used was 3g±0.5g. The constant temperature water bath was started to adjust the temperature of the reaction system to 30℃±5℃.

[0010] Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 92g±2g and the amount of terpineol is 8g±2g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml.

[0011] When the temperature inside the reaction flask drops to 30℃±5℃, the mixture of β-pinene and terpineol is added dropwise at a constant rate, and the temperature inside the reaction flask is controlled to be between 55℃ and 60℃ during the dropwise addition process.

[0012] Stop adding the reagent when the temperature inside the reaction flask reaches 55°C;

[0013] After the addition is complete, maintain the reaction system at a constant temperature of 40℃±5℃ for 2 hours;

[0014] The reaction solution was subjected to hydrolysis and washing treatment, and the toluene was removed from the reaction solution at 160℃±10℃.

[0015] The material is discharged after being evacuated to -0.092Mpa±0.02Mpa at 225℃±10℃.

[0016] As a preferred option, the following steps are included:

[0017] Take a 250ml three-necked reaction flask, add 90g of analytical grade AR toluene, and adjust the stirring speed of the reaction flask to 450r / min.

[0018] Analytical grade AR aluminum trichloride was added to the above reaction flask in one go, with an amount of 2.5g of aluminum trichloride. The constant temperature water bath was started to adjust the temperature of the reaction system to 25℃.

[0019] Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 90g and the amount of terpineol is 10g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml.

[0020] When the temperature inside the reaction flask drops to 25°C, the mixture of β-pinene and terpineol is added dropwise at a constant rate, and the temperature inside the reaction flask is controlled to be between 55°C and 60°C during the dropwise addition process.

[0021] Stop adding the reagent when the temperature inside the reaction flask reaches 55°C;

[0022] After the addition is complete, maintain the reaction system at a constant temperature of 35°C for 2 hours;

[0023] The reaction solution was subjected to hydrolysis and washing treatment, and toluene was removed from the reaction solution at 150°C.

[0024] The material is discharged after being vacuumed to -0.090 MPa at 215℃.

[0025] As a preferred method, the following steps are included: take a three-necked reaction flask with a capacity of 250 ml, add analytical grade AR toluene to it, the amount of toluene is 110 g, and adjust the stirring speed of the reaction flask to 550 r / min.

[0026] Analytical grade AR aluminum trichloride was added to the above reaction flask in one go, with an amount of 3.5g of aluminum trichloride. The constant temperature water bath was started to adjust the temperature of the reaction system to 35℃.

[0027] Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 94g and the amount of terpineol is 6g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml.

[0028] When the temperature inside the reaction flask drops to 35°C, a mixture of β-pinene and terpineol is added dropwise at a constant rate, while the temperature inside the reaction flask is controlled to be between 55°C and 60°C during the dropwise addition process.

[0029] Stop adding the reagent when the temperature inside the reaction flask reaches 55°C;

[0030] After the addition is complete, maintain the reaction system at a constant temperature of 45°C for 2 hours;

[0031] The reaction solution was subjected to hydrolysis and washing treatment, and the toluene was removed from the reaction solution at 170°C.

[0032] The material is discharged after being vacuumed to -0.094 MPa at 235℃.

[0033] As a preferred method, the following steps are included: take a three-necked reaction flask with a capacity of 250 ml, add analytical grade AR toluene to it, the amount of toluene is 100 g, and adjust the stirring speed of the reaction flask to 500 r / min;

[0034] Analytical grade AR aluminum trichloride was added to the above reaction flask in one go. The amount of aluminum trichloride used was 3g. The constant temperature water bath was started to adjust the temperature of the reaction system to 30℃.

[0035] Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 92g and the amount of terpineol is 8g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml.

[0036] When the temperature inside the reaction flask drops to 30°C, a mixture of β-pinene and terpineol is added dropwise at a constant rate, while the temperature inside the reaction flask is controlled to be between 55°C and 60°C during the dropwise addition process.

[0037] Stop adding the reagent when the temperature inside the reaction flask reaches 55°C;

[0038] After the addition is complete, maintain the reaction system at a constant temperature of 40°C for 2 hours;

[0039] The reaction solution was subjected to hydrolysis and washing treatment, and toluene was removed from the reaction solution at 160°C.

[0040] The material is discharged after being vacuumed to -0.092 MPa at 225℃.

[0041] As a preferred method, the hydrolysis and washing process is as follows: preheat the hot water to 95°C for later use, and start the four-stage washing vessel for stirring; for the first washing, use 95°C hot water, add 1kg of demulsifier to each vessel, stir for 25 minutes and let stand for 30 minutes; for the second, third and fourth washings, use hot water at 80-85°C, stir for 15 minutes and let stand for 25 minutes to separate the layers.

[0042] Preferably, the pH of the aqueous phase is set to 7-8 during the fourth water wash.

[0043] As a preferred method, the material is discharged after being evacuated to -0.092 MPa ± 0.02 MPa at 225℃ ± 10℃.

[0044] Pump the terpene mother liquor into the terpene mother liquor high-level tank and turn on the heat transfer oil to heat it slowly.

[0045] When toluene begins to distill out at 100°C, carefully observe the boiling situation in the vessel to prevent the material from overflowing. When the vessel temperature rises to 125°C, start adding the mother liquor dropwise until all the mother liquor has been added to the vessel.

[0046] Start heating up, reduce the heat transfer oil when it reaches 210℃, and completely shut off the heat transfer oil when the kettle temperature is 225℃±10℃. Evacuate to -0.092Mpa±0.02Mpa.

[0047] As a preferred method, nitrogen vacuum sampling and testing are used during material discharge. If the softening point is 22-28℃, the material is considered qualified for discharge.

[0048] Compared with the prior art, the present invention has the following advantages:

[0049] Because the double bond in the β-pinene molecule is located on the cycloalkane branch, it exhibits high reactivity during reactions. Grafting between β-pinene molecules is easy, meaning it readily forms large polymer molecules. Therefore, current production technology for β-pinene resin can only be used to produce high-softening-point terpene resins, typically with softening points between 110℃ and 140℃. Polymerization is achieved by adding a certain amount of terpineol to inhibit its polymerization activity and prevent the formation of large molecules, thus obtaining a product with the desired molecular size and a softening point between 22-28℃. Detailed Implementation

[0050] The specific embodiments of the present invention will be further described in detail to make the technical solution of the present invention easier to understand and master.

[0051] Example

[0052] This embodiment details the polymerization, washing, and distillation processes in the preparation of β-pinene liquid resin, and how to strictly follow the operating procedures to ensure the quality of the final product.

[0053] Aggregation operation steps

[0054] Before the polymerization reaction begins, prepare the following raw materials: 5700 kg toluene, 5520 kg β-pinene, 180 kg aluminum trichloride (60 kg per batch), and 480 kg terpineol.

[0055] Before mixing, use 200kg of imported β-pinene to replace the oil reservoir, release it through the mixing tank pipeline, stir the prepared turpentine oil for 30 minutes, let it stand for 30 minutes to separate the water, until the water is completely removed.

[0056] The treated turpentine is pumped into a high-level tank for later use.

[0057] Before starting the operation, check that the bottom valve of the polymerization reactor is closed, the bottom valves of the turpentine and toluene metering tanks are closed, and confirm that the exhaust gas venting system is unobstructed.

[0058] Pump 6000 kg of turpentine (added in three batches of 2000 kg each) and 5700 kg of toluene into the high-level metering tank and let it stand for 30 minutes to ensure that the water is drained completely.

[0059] Open the bottom valve of the toluene metering tank and let the anhydrous toluene flow into the polymerization reactor to ensure that the toluene is completely added so as not to affect the subsequent reaction process.

[0060] Start the agitator in the polymerization reactor and turn on the chilled water inlet valve and the cold brine pump, depending on the weather conditions. Once the toluene temperature inside the reactor drops to 35°C, turn off the brine pump and allow it to continue cooling naturally. If the outdoor temperature is low, the cooling system does not need to be activated.

[0061] Add 70 kg of catalyst (per reactor), ensuring accurate weighing before adding it all at once. If the reactor temperature does not rise significantly, turpentine can be added dropwise to initiate the reaction. The initial addition of turpentine should raise the reaction temperature to 60°C. Continue adding turpentine thereafter, lowering the temperature to 45°C each time it rises to 55°C, until all remaining turpentine has been added.

[0062] After the turpentine oil is added, maintain the reaction vessel at 40°C for 2 hours. During this time, regularly check the temperature of the reaction vessel to prevent excessive heating. After the turpentine oil addition is complete, continue to maintain the temperature for 30 minutes, then take a sample to observe the color of the reaction solution.

[0063] After holding at 40℃ for 2 hours, the material is discharged, completing the polymerization process.

[0064] Water washing operation steps

[0065] Transfer the material from the polymerization reactor to washing reactors #1, #2, and #3, and preheat the hot water to 95°C. Turn on the stirring system of the washing reactors to begin the first washing.

[0066] First wash: Use 95℃ hot water, add 1kg of demulsifier to each batch, stir for 25 minutes, and let stand for 30 minutes before separation begins.

[0067] Second wash: Use 90℃ hot water, stir for 15 minutes, let stand for 25 minutes until the layers separate.

[0068] Third wash: Use 85℃ hot water, stir for 15 minutes, let stand for 25 minutes until the layers separate.

[0069] Fourth wash: Use 80℃ hot water, stir for 15 minutes, let stand for 25 minutes to separate the layers.

[0070] After the fourth wash, the pH value of the aqueous phase is tested to ensure it is within the range of 7-8.

[0071] Pay special attention to the turbidity of oil and alcohol substances in the water during the first stratification, and strictly control the observation of the stratification interface.

[0072] Samples were taken and tested promptly after the first water wash, and the reaction yield was calculated.

[0073] After the fourth water wash, samples were taken and colorimetric tests were conducted to ensure that the mother liquor met the color standard.

[0074] Product distillation operation steps

[0075] Before distillation, check the bottom valve and discharge valve of the distillation vessel to ensure they are closed.

[0076] Open the feed valve and the condenser circulating water inlet valve, open the condenser vent valve, and close the vent valve after the condenser is full of water.

[0077] 2900 kg of terpene mother liquor was pumped into the high-level tank of terpene mother liquor, and the solution volume was recorded.

[0078] Start the heat transfer oil heating system and slowly heat the distillation vessel.

[0079] When the temperature rises to 100℃, start observing the distillation of toluene to avoid violent boiling in the reaction vessel and prevent solution splashing.

[0080] When the temperature rises to 125℃, the remaining mother liquor is gradually added dropwise until all 11,000 kg of mother liquor has been added.

[0081] Then, when the temperature reaches 210°C, the heat transfer oil system is turned off and heating continues to 230°C.

[0082] The heat transfer oil was completely shut off at 230℃, and after heating was completed, a vacuum was drawn to -0.092MPa to ensure the smooth progress of the distillation process.

[0083] Nitrogen gas is used to de-vacuum the product, and samples are taken for testing during the decompression process to ensure that the softening point of the product is 22-28℃.

[0084] Adjust the product's color as needed to ensure the final product's color is within the specified range (<5 colors). If the color is unacceptable, add an appropriate amount of decolorizing agent for treatment.

[0085] Polymerization process: Ensure the reaction temperature is stable at 55℃ to guarantee the complete reaction of each batch of product.

[0086] Washing process: The temperature and stirring time of each wash are strictly controlled to ensure that the washing effect meets the requirements, the pH value of the product is between 7 and 8, and the color of the final aqueous phase meets the standard.

[0087] Distillation process: During distillation, the final temperature is controlled to not exceed 240℃ and the softening point is ensured to be 25℃. The quality of the final product is guaranteed by controlling the vacuum degree and colorimetric method.

[0088] Example 2

[0089] A method for preparing a β-pinene liquid resin includes the following steps:

[0090] Raw material preparation: 5700kg toluene, 5520kg β-pinene, 180kg aluminum trichloride (60kg per batch), 480kg terpineol;

[0091] Turpentine pretreatment: Use 200kg of imported β-pinene to replace the oil reservoir, stir the turpentine for 30 minutes, and let it stand for 30 minutes to separate the water, ensuring that the water is completely removed.

[0092] After treatment with turpentine, it is pumped into a high-level tank for later use.

[0093] Pre-operation checks: Check that the bottom valve of the polymerization reactor and the bottom valve of the toluene metering tank are closed, and confirm that the exhaust gas venting system is unobstructed. Pump 6000 kg of turpentine (added in three batches of 2000 kg each) and 5700 kg of toluene into the high-level metering tank, and let it stand for 30 minutes to drain the water completely.

[0094] Polymerization process: Open the bottom valve of the toluene metering tank and let anhydrous toluene flow into the polymerization reactor, ensuring complete addition. Start the agitator and, depending on the weather conditions, activate the chilled water and cold brine systems to maintain the reactor temperature at approximately 35°C. Add 70 kg of aluminum trichloride catalyst, ensuring the reaction temperature gradually increases. If the reaction temperature does not rise, turpentine can be added dropwise to initiate the reaction. Initially add turpentine to 60°C, maintaining the temperature between 45°C and 55°C after each addition until the remaining turpentine has been completely added. After adding turpentine, maintain the reactor at 40°C for 2 hours, and check the temperature regularly to prevent excessively rapid heating.

[0095] Discharge: After the reaction is complete, discharge begins, completing the polymerization process.

[0096] Water washing operation steps

[0097] Preparation before water washing: Transfer the material in the polymerization reactor to water washing reactors 1#, 2#, and 3#, and preheat the hot water to 95℃.

[0098] Washing process: First wash: Use 95℃ hot water, add 1kg of demulsifier to each batch, stir for 25 minutes, let stand for 30 minutes until separation occurs. Second wash: Use 90℃ hot water, stir for 15 minutes, let stand for 25 minutes until separation occurs. Third wash: Use 85℃ hot water, stir for 15 minutes, let stand for 25 minutes until separation occurs. Fourth wash: Use 80℃ hot water, stir for 15 minutes, let stand for 25 minutes until separation occurs.

[0099] Quality control: Test the pH of the aqueous phase after the fourth wash to ensure it is between 7 and 8. Pay special attention to the turbidity of oil and alcohol substances during the first separation, and strictly control the separation interface. Take samples for analysis promptly after the first wash and calculate the reaction yield.

[0100] Color and compliance: Samples were taken and colorimetric tests were performed after the fourth water wash to ensure that the mother liquor met the color standard.

[0101] Product distillation operation steps

[0102] Preparation before distillation: Check the bottom valve and discharge valve of the distillation vessel to ensure they are closed. Open the feed valve and condenser circulating water inlet valve, open the condenser vent valve, and close the vent valve after the condenser is full of water.

[0103] Mother liquor addition: Pump 2900 kg of terpene mother liquor into the terpene mother liquor high-level tank and record the solution volume.

[0104] Heating process: Start the heat transfer oil heating system and slowly heat the distillation vessel. When the temperature reaches 100℃, begin observing the distillation of toluene to avoid violent boiling. When the temperature reaches 125℃, gradually add the remaining mother liquor dropwise until all 11,000 kg of mother liquor has been added.

[0105] Distillation control: When the temperature reaches 210℃, shut off the heat transfer oil system and continue heating to 230℃. At 230℃, completely shut off the heat transfer oil, stop heating, and evacuate to -0.092MPa.

[0106] Vacuum treatment and testing: The vacuum is released using nitrogen, and samples are taken for testing during the decompression process to ensure the product's softening point is between 22-28℃. The product color is adjusted as needed to ensure the final product color meets the standard (<5 colors). If color difference exists, an appropriate amount of decolorizing agent can be added.

[0107] During polymerization, the reaction temperature should be maintained at approximately 55°C, and the reaction time should be sufficient to ensure complete reaction of each batch of product, avoiding temperature fluctuations. In cold weather, the cooling system operation can be adjusted appropriately or the flow rate of the cold brine can be reduced.

[0108] During water washing, the temperature and stirring time must be precisely controlled each time to avoid the effect of excessively low or high temperatures, and to ensure that the pH value and color of the aqueous phase are within the specified range.

[0109] During distillation, the final temperature should be strictly controlled to not exceed 240℃ to avoid affecting product quality. Ensure the softening point is controlled at around 25℃, and optimize the final product by adjusting the vacuum level and using colorimetric methods.

[0110] Example 3

[0111] A method for preparing a β-pinene liquid resin includes the following steps:

[0112] Raw material preparation: Toluene: 5700 kg, β-pinene: 5520 kg, aluminum trichloride catalyst: 180 kg (60 kg per batch), terpineol: 480 kg.

[0113] Turpentine oil pretreatment: Use a 200kg imported β-pinene displacement tank, stir for 30 minutes, let stand for 30 minutes to separate water, ensuring water removal. The treated turpentine oil is then pumped into a high-level tank for later use.

[0114] Pre-operation checks: Check whether the bottom valve of the polymerization reactor is closed, whether the bottom valves of the toluene and turpentine metering tanks are closed, and confirm that the exhaust gas venting system is unobstructed.

[0115] Polymerization process: Addition of turpentine and toluene: Pump 6000 kg of turpentine (added in three batches of 2000 kg each) and 5700 kg of toluene into the high-level tank and let it stand for 40 minutes to ensure complete drainage. Open the bottom valve of the toluene metering tank and let the anhydrous toluene flow into the polymerization reactor, ensuring complete addition. Start the agitator and adjust the cooling system according to the outside weather temperature to maintain the reactor temperature at 30℃-35℃.

[0116] Catalyst addition: Add 60 kg of aluminum trichloride catalyst (per batch), ensuring accurate weighing before adding in one go. If the temperature does not rise significantly, turpentine can be added dropwise to initiate the reaction. Initially add turpentine to 65°C, and then after each subsequent addition, gradually raise the temperature to 60°C, then maintain it between 45°C and 55°C until all the turpentine has been added.

[0117] Heat preservation stage: After the turpentine is added, maintain the temperature at 45℃ and keep it warm for 1 hour to prevent the temperature from rising too quickly.

[0118] End and Discharge: After the reaction is complete, maintain the temperature at 40℃ and continue to keep it at that temperature for 1 hour. Once the temperature stabilizes, begin discharging to complete the polymerization process.

[0119] Water washing operation steps

[0120] Preparation before washing: Transfer the material in the polymerization reactor to washing reactors 1#, 2#, and 3#, and preheat the hot water to 90℃.

[0121] Washing process: First wash: Use 90℃ hot water, add 1.5kg of demulsifier to each batch, stir for 20 minutes, let stand for 35 minutes until separation occurs. Second wash: Use 85℃ hot water, stir for 20 minutes, let stand for 30 minutes until separation occurs. Third wash: Use 80℃ hot water, stir for 20 minutes, let stand for 30 minutes until separation occurs. Fourth wash: Use 75℃ hot water, stir for 20 minutes, let stand for 30 minutes until separation occurs.

[0122] Quality control: Monitor the pH of the aqueous phase to ensure it is between 7 and 8. Observe the turbidity of oil and alcohol substances during the first layer separation to ensure the stability of the layer interface. Take samples after each water wash and analyze them to calculate the reaction yield.

[0123] Final inspection: After the fourth water wash, a colorimetric test is performed to ensure that the color of the mother liquor meets the standard and the color value is within the specified range.

[0124] Product distillation operation steps

[0125] Preparation before distillation: Check the bottom valve and discharge valve of the distillation vessel to ensure they are closed. Start the condenser circulating water system and check the vent valve to ensure the condenser system is operating normally.

[0126] Mother liquor addition: Pump 2900 kg of terpene mother liquor into the terpene mother liquor high-level tank and record the solution volume.

[0127] Heating process: Start the heat transfer oil heating system and slowly heat the distillation vessel to avoid a sudden temperature rise. When the temperature reaches 110℃, observe the toluene distillation to prevent violent boiling within the reaction vessel. When the temperature reaches 130℃, gradually add the remaining mother liquor dropwise until all 11,000 kg of mother liquor has been added.

[0128] Distillation control: When the temperature reaches 215℃, shut off the heat transfer oil system and continue heating to 230℃. At 230℃, completely shut off the heat transfer oil system, stop heating, and evacuate to -0.09MPa to ensure the smooth progress of the distillation process.

[0129] Vacuum treatment and product testing: Use nitrogen to release the vacuum, ensuring the product's softening point remains between 22℃ and 30℃ during decompression. Adjust the product color as needed to ensure the final product color meets the color standard (<5 colors). If the color is unacceptable, add an appropriate amount of decolorizing agent.

[0130] Performance testing experiment

[0131] Experimental steps:

[0132] Take a sample of the β-pinene liquid resin from the above embodiment and ensure its purity and uniformity.

[0133] Place the resin sample in the sample chamber of the softening point tester, or use a glass tube method device for measurement.

[0134] A temperature control device is installed to gradually increase the temperature of the sample during the heating process.

[0135] The sample state was recorded every 1°C to observe the temperature at which it changed from a solid state to a softened state.

[0136] Record the temperature value immediately when the sample begins to show signs of softening (such as deformation or becoming viscous).

[0137] The experiment was repeated three times, and the softening point temperature was recorded and the average value was calculated each time. The results are shown in Table 1 below.

[0138] Table 1 Experimental Data Recording Table

[0139] Experiment number Heating temperature (°C) Sample status Remark 1 22.0 Start to soften Initial deformation 2 22.5 Continue to soften Slightly sticky 3 23.0 Completely softened No obvious hardness 4 23.5 Slightly soft There is slight flow on the surface. 5 24.0 Soften completely The sample softened completely 6 24.5 Slight liquidity The sample was significantly deformed. 7 25.0 Completely softened No visible hardness 8 25.5 No significant changes Softening complete 9 26.0 Completely softened Continue to flow 10 26.5 Completely softened High temperature changes 11 27.0 Completely softened The sample has no hardness 12 27.5 Completely softened The sample has no hardness

[0140] The experimental data show that β-pinene liquid resin begins to soften and fully softens between 22.0℃ and 27.5℃, which is consistent with the expected softening point range (22℃-28℃).

[0141] Average softening point: According to the experimental results, the softening point of β-pinene liquid resin is 24.0℃ (this value is the average of multiple experiments).

[0142] Conclusion: Experiments verified that the softening point of β-pinene liquid resin is between 22℃ and 28℃, which is consistent with theoretical expectations. Experimental data support that the softening point of this resin material is within the expected range and is suitable for relevant applications.

[0143] Of course, the above are merely typical examples of the present invention. Besides these, the present invention can have many other specific embodiments. All technical solutions formed by equivalent substitution or equivalent transformation fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing a β-pinene liquid resin, characterized in that... This includes the following steps: Take a three-necked reaction flask with a capacity of 250 ml, add analytical grade AR toluene to it, the amount of toluene is 100 g ± 10%, and adjust the stirring speed of the reaction flask to 500 r / min ± 10%. Analytical grade AR aluminum trichloride was added to the above reaction flask in one go. The amount of aluminum trichloride used was 3g±0.5g. The constant temperature water bath was started to adjust the temperature of the reaction system to 30℃±5℃. Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 92g±2g and the amount of terpineol is 8g±2g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml. When the temperature inside the reaction flask drops to 30℃±5℃, the mixture of β-pinene and terpineol is added dropwise at a constant rate, and the temperature inside the reaction flask is controlled to be between 55℃ and 60℃ during the dropwise addition process. Stop adding the reagent when the temperature inside the reaction flask reaches 55°C; After the addition is complete, maintain the reaction system at a constant temperature of 40℃±5℃ for 2 hours; The reaction solution was subjected to hydrolysis and washing treatment, and the toluene was removed from the reaction solution at 160℃±10℃. The material is discharged after being evacuated to -0.092Mpa±0.02Mpa at 225℃±10℃.

2. The method for preparing β-pinene liquid resin according to claim 1, characterized in that... This includes the following steps: Take a 250ml three-necked reaction flask, add 90g of analytical grade AR toluene, and adjust the stirring speed of the reaction flask to 450r / min. Analytical grade AR aluminum trichloride was added to the above reaction flask in one go, with an amount of 2.5g of aluminum trichloride. The constant temperature water bath was started to adjust the temperature of the reaction system to 25℃. Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 90g and the amount of terpineol is 10g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml. When the temperature inside the reaction flask drops to 25°C, the mixture of β-pinene and terpineol is added dropwise at a constant rate, and the temperature inside the reaction flask is controlled to be between 55°C and 60°C during the dropwise addition process. Stop adding the reagent when the temperature inside the reaction flask reaches 55°C; After the addition is complete, maintain the reaction system at a constant temperature of 35°C for 2 hours; The reaction solution was subjected to hydrolysis and washing treatment, and toluene was removed from the reaction solution at 150°C. The material is discharged after being vacuumed to -0.090 MPa at 215℃.

3. The method for preparing β-pinene liquid resin as described in claim 1, characterized in that... This includes the following steps: Take a 250ml three-necked reaction flask, add analytical grade AR toluene (110g), and adjust the stirring speed of the reaction flask to 550r / min. Analytical grade AR aluminum trichloride was added to the above reaction flask in one go, with an amount of 3.5g of aluminum trichloride. The constant temperature water bath was started to adjust the temperature of the reaction system to 35℃. Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 94g and the amount of terpineol is 6g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml. When the temperature inside the reaction flask drops to 35°C, a mixture of β-pinene and terpineol is added dropwise at a constant rate, while the temperature inside the reaction flask is controlled to be between 55°C and 60°C during the dropwise addition process. Stop adding the reagent when the temperature inside the reaction flask reaches 55°C; After the addition is complete, maintain the reaction system at a constant temperature of 45°C for 2 hours; The reaction solution was subjected to hydrolysis and washing treatment, and the toluene was removed from the reaction solution at 170°C. The material is discharged after being vacuumed to -0.094 MPa at 235℃.

4. The method for preparing β-pinene liquid resin according to claim 1, characterized in that... This includes the following steps: Take a 250ml three-necked reaction flask, add 100g of analytical grade AR toluene, and adjust the stirring speed of the reaction flask to 500r / min. Analytical grade AR aluminum trichloride was added to the above reaction flask in one go. The amount of aluminum trichloride used was 3g. The constant temperature water bath was started to adjust the temperature of the reaction system to 30℃. Mix 98% β-pinene with fragrance-grade terpineol, wherein the amount of β-pinene is 92g and the amount of terpineol is 8g, and then pour the mixture into a constant pressure dropping funnel with a capacity of 125ml. When the temperature inside the reaction flask drops to 30°C, a mixture of β-pinene and terpineol is added dropwise at a constant rate, while the temperature inside the reaction flask is controlled to be between 55°C and 60°C during the dropwise addition process. Stop adding the reagent when the temperature inside the reaction flask reaches 55°C; After the addition is complete, maintain the reaction system at a constant temperature of 40°C for 2 hours; The reaction solution was subjected to hydrolysis and washing treatment, and toluene was removed from the reaction solution at 160°C. The material is discharged after being vacuumed to -0.092 MPa at 225℃.

5. The method for preparing β-pinene liquid resin according to claim 1, characterized in that, The method for hydrolysis and washing is as follows: heat the pre-used hot water to 95℃ for later use, and start the four-stage washing kettle for stirring; for the first washing, use 95℃ hot water, add 1kg of demulsifier to each kettle, stir for 25min and let stand for 30min; for the second, third and fourth washing, use hot water at 80-85℃, stir for 15min and let stand for 25min to separate into layers.

6. The method for preparing β-pinene liquid resin according to claim 5, characterized in that, During the fourth water wash, the pH of the aqueous phase is adjusted to 7-8.

7. The method for preparing β-pinene liquid resin according to claim 1, characterized in that, The method for discharging material after vacuuming to -0.092Mpa±0.02Mpa at 225℃±10℃ is as follows: Pump the terpene mother liquor into the terpene mother liquor high-level tank and turn on the heat transfer oil to heat it slowly. When toluene begins to distill out at 100°C, carefully observe the boiling situation in the vessel to prevent the material from overflowing. When the vessel temperature rises to 125°C, start adding the mother liquor dropwise until all the mother liquor has been added to the vessel. Start heating up, reduce the heat transfer oil when it reaches 210℃, and completely shut off the heat transfer oil when the kettle temperature is 225℃±10℃. Evacuate to -0.092Mpa±0.02Mpa.

8. The method for preparing β-pinene liquid resin according to claim 7, characterized in that, During the discharge process, nitrogen gas is used for vacuum sampling and testing. If the softening point is 22-28℃, the material is considered qualified for discharge.