Combined cumquat and preparation method and application thereof

Abstract

The invention discloses combined cumquat and a preparation method and application thereof, and belongs to the technical field of combined cumquat preparation. The preparation method comprises the following steps: adding di-tert-butyl peroxide into isopropyl benzene at the temperature of more than or equal to 130 DEG C and less than 140 DEG C for reaction; the molar ratio of the cumene to the di-tert-butyl peroxide is (2: 0.6)-(2: 1.4), the adding speed of the di-tert-butyl peroxide is 1s / drop to 2s / drop, the reaction temperature does not exceed 150 DEG C, and the reaction time is not less than 4 hours. The method is simple to operate, relatively low in cost, relatively short in reaction time, free of wastewater generation and environment-friendly, only one initiator is needed, and combined cumyl chloride with relatively high purity can be obtained through the method. The obtained combined catalyst can be used for flame-retardant synergism, high-molecular modification or initiation of high-temperature polymer reaction and the like.

Description

Technical Field

[0001] The present invention relates to the technical field of co-drying, and in particular to a co-drying and a preparation method and application thereof. Background Art

[0002] 2,3-Dimethyl-2,3-diphenylbutane, also known as 2,3-dimethyl-2,3-diphenylbutane. The carbon-carbon bond between the quaternary carbon atoms in the 2,3-dimethyl-2,3-diphenylbutane molecule is not very stable and is easily dissociated into free radicals. Based on this characteristic, 2,3-dimethyl-2,3-diphenylbutane is widely used as a new type of additive in flame retardant enhancement, polymer modification, and initiation of high-temperature polymer reactions, among which the application as a flame retardant enhancer is more noteworthy.

[0003] In order to make the polymer obtain flame retardant properties, one direction is to add additives with flame retardant ability, and the other direction is to introduce side chains with flame retardant effect into the main chain of the polymer, but the cost of introducing side chains is high and the introduction efficiency is not ideal. The current market-oriented method is to add additives, especially organic halides. The flame retardant effect of halides is positively correlated with the content of halogen elements. Therefore, in order to obtain better flame retardant effects, a large amount of organic halides will be added to the polymer, but a large amount of halides will affect the mechanical strength and light stability of the polymer. The use of dimethicone as a synergist can not only reduce the impact on polymer properties, but also obtain better flame retardant properties with less organic halides added. The flame retardant synergistic mechanism of dimethicone is: at high temperature, dimethicone is cracked into dimethylphenyl tertiary carbon radicals, and together with the free radicals generated by the cracking of other organic halides, it synergistically captures the active free radicals generated during combustion, making the combustion reaction chain unable to proceed and thus achieving a flame retardant effect.

[0004] At present, there are two main methods for synthesizing ligand. One is to use α-methylstyrene as raw material to synthesize intermediate halides, and then react with active metals to synthesize grignard reagents, and then couple to synthesize ligand. The problems with this method are that the synthesized halides are unstable and easily decomposed at room temperature; α-methylstyrene is easy to polymerize, which increases the viscosity of the reaction liquid, increases the difficulty of product separation, and cannot be reused; the reaction requires the use of active metals such as zinc and magnesium, which is costly and difficult to achieve industrialization.

[0005] Another method is to use cumene as a raw material, generate free radicals with a free radical initiator, and then couple cumene to generate cumene free radicals. The free radical initiators used are mostly dibenzoyl peroxide and di-tert-butyl peroxide, and other low-temperature free radical initiators are required. Compared with the halogenation coupling reaction product, this method is easier to separate and more suitable for industrial production, but during the reaction, the accumulation of by-products benzoic acid or isopropanol will reduce the boiling point, the decomposition efficiency of peroxide will become lower and lower, and after the reaction is completed, the reaction liquid has too many components, and the reuse process of initiators and raw materials is relatively complicated or cannot be reused; the reaction time is long, usually more than 10 hours.

[0006] In view of this, the present invention is proposed. Summary of the invention

[0007] The object of the present invention is to provide a kind of joint dry and its preparation method and application, so as to solve or improve the above-mentioned technical problems.

[0008] The present invention can be implemented like this: In a first aspect, the present invention provides a method for preparing linalool, comprising the following steps: adding di-tert-butyl peroxide to cumene at a temperature of ≥130°C and <140°C for reaction; The molar ratio of isopropylbenzene to di-tert-butyl peroxide is 2:0.6 to 2:1.4, the addition rate of di-tert-butyl peroxide is 1s / drop to 2s / drop, the reaction temperature does not exceed 150°C, and the reaction time is not less than 4h.

[0009] In an optional embodiment, cumene is heated to ≥100°C and <140°C in an oil bath.

[0010] In an optional embodiment, the cumene heated in an oil bath to ≥100°C and <140°C is first dehydrated, the temperature of the dehydrated cumene is controlled to be ≥130°C and <140°C, and then di-tert-butyl peroxide is added.

[0011] In an alternative embodiment, the reaction temperature is ≥135°C and <150°C.

[0012] In an optional embodiment, the reaction temperature is 140°C to 145°C.

[0013] In an optional embodiment, the temperature of the reaction solution is maintained at not less than 125° C. during the addition of di-tert-butyl peroxide.

[0014] In an optional embodiment, the reaction time is 4h~6h.

[0015] In an optional embodiment, the method further comprises: crystallizing the reaction solution after the reaction is completed, and performing solid-liquid separation to obtain a solid.

[0016] In an optional embodiment, the method further comprises: washing and drying the solid.

[0017] In an optional embodiment, the method further comprises: using the liquid obtained from the solid-liquid separation as a raw material for the next synthesis of the co-drying agent.

[0018] In an optional embodiment, the method further comprises: fractionating the distillate in the reaction process to obtain fractions, and recycling the fractions.

[0019] In a second aspect, the present invention provides a kind of lianku prepared by the preparation method of any one of the aforementioned embodiments.

[0020] In an optional embodiment, the joint has at least one of the following characteristics: Feature 1: The yield of Lianku is not less than 16%; Feature 2: The purity of Lianku is not less than 96%.

[0021] In a third aspect, the present invention provides an application of the aforementioned embodiment, such as flame retardant enhancement, polymer modification or initiation of high temperature polymer reaction.

[0022] The beneficial effects of the present invention include: The present invention uses di-tert-butyl peroxide as the only free radical initiator and controls the reaction temperature, material drop rate and reaction time to obtain a high-purity coke. The method has simple steps, and both by-products and unreacted raw materials can be effectively reused, which is conducive to cost saving. The method does not generate wastewater and is environmentally friendly. The obtained coke can be used for flame retardant enhancement, polymer modification or initiation of high-temperature polymer reaction. DETAILED DESCRIPTION

[0023] 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.

[0024] The following is a detailed description of the invention's preparation method and application.

[0025] The invention provides a method for preparing a cyclopentane, which comprises the following steps: adding di-tert-butyl peroxide to isopropylbenzene at a temperature of ≥130°C and <140°C for reaction.

[0026] The molar ratio of isopropylbenzene to di-tert-butyl peroxide is 2:0.6 to 2:1.4, the addition rate of di-tert-butyl peroxide is 1s / drop to 2s / drop, the reaction temperature does not exceed 150°C, and the reaction time is not less than 4h.

[0027] By using di-tert-butyl peroxide as the only free radical initiator and controlling the reaction temperature, material drop rate and reaction time, a high-purity coke can be obtained. The method is simple in steps, and by-products and unreacted raw materials can be effectively reused, which is conducive to cost saving. In addition, the method does not generate wastewater and is environmentally friendly.

[0028] In some embodiments, cumene may be heated to ≥100° C. and <140° C. in an oil bath. During the process, mechanical stirring may be performed to ensure uniform heating of cumene.

[0029] In some embodiments, cumene heated to ≥100°C and <140°C in an oil bath is first subjected to a water removal treatment, the temperature of the cumene after water removal is controlled to be ≥130°C and <140°C, and then di-tert-butyl peroxide is added.

[0030] Exemplarily, the temperature for removing water may be 100°C, 105°C, 110°C, 115°C, 120°C, 125°C, 130°C, 135°C or 139°C, etc., or other values ​​within the range of ≥100°C and <140°C.

[0031] By removing water, it is possible to avoid that the water in the reaction system affects the reaction rate (specifically, reduces the reaction rate) when di-tert-butyl peroxide is added dropwise, thereby reducing the utilization rate of di-tert-butyl peroxide.

[0032] Exemplarily, the water removal time can be adjusted according to actual conditions. Taking the oil bath temperature as 105° C. as an example, the water removal time can be 0.5 h.

[0033] Exemplarily, after water removal, the temperature of cumene can be controlled to 130° C., 131° C., 132° C., 133° C., 134° C., 135° C., 136° C., 137° C., 138° C., or 139° C., etc., or other values ​​within the range of ≥130° C. and <140° C. In some preferred embodiments, after water removal, the temperature of cumene can be controlled to 130° C. to 135° C.

[0034] In the present invention, the molar ratio of isopropylbenzene to di-tert-butyl peroxide can be 2:0.6 to 2:1.4, such as 2:0.6, 2:0.7, 2:0.8, 2:0.9, 2:1, 2:1.1, 2:1.2, 2:1.3 or 2:1.4, or other values ​​within the range of 2:0.6 to 2:1.4.

[0035] The addition rate of di-tert-butyl peroxide can be 1 s / drop to 2 s / drop, such as 1 s / drop, 1.5 s / drop or 2 s / drop.

[0036] If the addition speed of di-tert-butyl peroxide is too fast, more di-tert-butyl peroxide will be decomposed, greatly reducing the utilization rate of di-tert-butyl peroxide.

[0037] In some embodiments, the reaction temperature of cumene and di-tert-butyl peroxide is ≥135°C and <150°C. Exemplarily, the reaction temperature of cumene and di-tert-butyl peroxide can be 135°C, 138°C, 140°C, 142°C, 145°C, 148°C or 149°C, etc., or other values ​​within the range of ≥135°C and <150°C. In some preferred embodiments, the reaction temperature of cumene and di-tert-butyl peroxide is 140°C to 145°C.

[0038] During the process of adding di-tert-butyl peroxide, the temperature of the reaction solution is maintained at not less than 125°C to ensure effective reaction of cumene and di-tert-butyl peroxide. In some embodiments, the temperature of the reaction solution can be maintained at ≥125°C and <140°C.

[0039] In some embodiments, the reaction time of isopropylbenzene and di-tert-butyl peroxide is 4h~6h, such as 4h, 4.5h, 5h, 5.5h or 6h, etc., and can also be other values ​​within the range of 4h~6h. In other embodiments, it can also be confirmed based on the residual amount of di-tert-butyl peroxide after the reaction, for example, the reaction can be stopped when the content of di-tert-butyl peroxide is less than 1wt%.

[0040] By reacting isopropylbenzene with di-tert-butyl peroxide, the reaction product contains dibutyl peroxide.

[0041] Furthermore, the reaction liquid after the reaction is completed can be crystallized and separated into solid and liquid to obtain a solid. The solid is a condensed solid.

[0042] Among them, crystallization is achieved by cooling, and solid-liquid separation can be achieved by filtration and other methods.

[0043] Furthermore, the solid is washed and dried to remove other substances attached to the surface of the solid.

[0044] The washing agent used for washing may include at least one of alcohols (such as methanol or ethanol) and ethyl acetate. Drying may be performed by drying.

[0045] The purity of the dimethoate prepared by the method provided by the present invention is not less than 96%, such as 96.92% to 98.54%.

[0046] In addition, in the method provided by the present invention, the liquid obtained by solid-liquid separation can also be used as a raw material for the next synthesis of coke.

[0047] Furthermore, the distillate in the preparation process can also be fractionated to obtain fractions, which include di-tert-butyl peroxide, isopropylbenzene and isopropyl alcohol.

[0048] The above fractions can be recycled, for example, di-tert-butyl peroxide and isopropylbenzene can be used as raw materials for the next synthesis of dibutyl peroxide, and isopropyl alcohol can be further used to synthesize di-tert-butyl peroxide.

[0049] In the above, compared with using halides to prepare Grignard reagents and then coupling to synthesize the quenching agent, the solution provided by the present invention has simpler steps, only one step of reaction, and the reaction does not involve halides, and there will be no situation where halides decompose at room temperature or under heating, which will not reduce the utilization rate of raw materials and increase the difficulty of product separation. In addition, the solution provided by the present invention does not require the use of active metal catalysts, saving costs.

[0050] Compared with the free radical coupling reaction that also uses peroxide in the prior art, the scheme provided by the present invention uses only a free radical initiator, the reaction solution composition is simpler, and by raising the temperature, the reaction rate is increased, and the reaction time of more than ten hours is not required. At the same time, the generated isopropanol byproduct can be fractionated out, and the coupling efficiency is further improved. In addition, the reaction solution and the distillate of the present invention can be reused. Since the isopropanol is fractionated out, there is almost only unreacted isopropylbenzene in the reaction solution, which can be directly used as the raw material for the next synthesis. After the distillate is fractionated, the raw material isopropylbenzene, di-tert-butyl peroxide and isopropyl alcohol can be obtained, wherein the isopropyl alcohol can be converted into di-tert-butyl peroxide. The washing reagent for washing the crude product can also be reused, and there is almost no waste water generation in actual production, and there is no three wastes treatment.

[0051] Correspondingly, the present invention provides a kind of lianku prepared by the above-mentioned preparation method.

[0052] In some embodiments, the yield of the linked dry is not less than 16%.

[0053] In some embodiments, the purity of the distilled water is not less than 96%.

[0054] In addition, the present invention also provides an application of the above-mentioned co-curing agent, for example, it can be used for flame retardant enhancement, polymer modification or initiation of high-temperature polymer reaction, etc.

[0055] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.

[0056] Example 1 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0057] S2: After the water is removed, the temperature is raised to 135°C, and 210 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:1.4) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. The temperature of the reaction solution is maintained at 130°C during the addition.

[0058] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0059] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0060] The yield of the above-mentioned combined product is 18.43% and the purity is 96.92%.

[0061] Example 2 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0062] S2: After the water is removed, the temperature is raised to 135°C, and 180 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:1.2) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. The temperature of the reaction solution is maintained at 130°C during the addition.

[0063] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0064] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0065] The yield of the above-mentioned combined product is 21.70% and the purity is 98.54%.

[0066] That is, the difference between this embodiment and embodiment 1 is that the molar ratio of cumene to di-tert-butyl peroxide is different.

[0067] Example 3 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0068] S2: After the water is removed, the temperature is raised to 135°C, and 150 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:1) is slowly added dropwise using a constant pressure dropping funnel at a rate of 1 s / drop. The temperature of the reaction solution is maintained at 130°C during the addition.

[0069] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0070] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0071] The yield of the above-mentioned combined product is 22.20% and the purity is 98.27%.

[0072] That is, the difference between this embodiment and embodiment 1 is that the molar ratio of cumene to di-tert-butyl peroxide is different.

[0073] Example 4 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0074] S2: After the water is removed, the temperature is raised to 135°C, and 120 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:0.8) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. The temperature of the reaction solution is maintained at 130°C during the addition.

[0075] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0076] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0077] The yield of the above-mentioned combined product is 26.29% and the purity is 98.44%.

[0078] That is, the difference between this embodiment and embodiment 1 is that the molar ratio of cumene to di-tert-butyl peroxide is different.

[0079] Example 5 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0080] S2: After the water removal is completed, the temperature is raised to 135°C, and 90 g of di-tert-butyl peroxide (the molar ratio of isopropylbenzene to di-tert-butyl peroxide is 2:0.6) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. During the addition, the temperature of the reaction solution is maintained at 130°C.

[0081] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0082] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0083] The yield of the above-mentioned combined product is 16.01% and the purity is 98.03%.

[0084] That is, the difference between this embodiment and embodiment 1 is that the molar ratio of cumene to di-tert-butyl peroxide is different.

[0085] Example 6 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 100°C, and remove water for 1 hour.

[0086] S2: After the water removal is completed, the temperature is raised to 130°C, and 120 g of di-tert-butyl peroxide (the molar ratio of isopropylbenzene to di-tert-butyl peroxide is 2:0.8) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 2s / drop. During the addition, the reaction liquid temperature is maintained at 125°C.

[0087] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 135°C and the reaction is carried out for 6 hours.

[0088] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the first suction filtration is performed. The solid obtained after the first suction filtration is added to 100 mL of ethanol and stirred for 1 hour, and the second suction filtration is performed. The solid obtained after the second suction filtration is dried to obtain the product Lianku.

[0089] Example 7 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the spike-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 135°C, and remove water for 0.2 h.

[0090] S2: After the water removal is completed, the temperature is raised to 139°C, and 120 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:0.8) is slowly added dropwise using a constant pressure dropping funnel at a rate of 1.5 drops. The temperature of the reaction solution is maintained at 139°C during the addition.

[0091] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 149°C and the reaction is carried out for 4 hours.

[0092] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of ethyl acetate and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0093] Comparative Example 1 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0094] S2: After the water is removed, the temperature is raised to 135°C, and 120 g of di-tert-butyl peroxide is directly added (the molar ratio of isopropylbenzene to di-tert-butyl peroxide is 2:0.8).

[0095] S3: After the addition of di-tert-butyl peroxide is complete, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0096] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0097] The yield of the above-mentioned combined product is 5.87% and the purity is 97.32%.

[0098] That is, the difference between this comparative example and Example 4 is that di-tert-butyl peroxide is added at one time.

[0099] Comparative Example 2 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0100] S2: After the water is removed, the temperature is raised to 135°C, and 40 g of di-tert-butyl peroxide is added at a time every hour, and a total of 120 g of di-tert-butyl peroxide is added over 2 hours (the molar ratio of isopropylbenzene to di-tert-butyl peroxide is 2:0.8).

[0101] S3: After the addition of di-tert-butyl peroxide is complete, the temperature is raised to 145°C and the reaction is carried out for 4 hours.

[0102] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0103] The yield of the above-mentioned combined product is 7.83% and the purity is 95.93%.

[0104] That is, the difference between this comparative example and Example 4 is that di-tert-butyl peroxide is not added dropwise continuously but is added in three times.

[0105] Comparative Example 3 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0106] S2: After the water removal is completed, the temperature is raised to 110°C, and 120 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:0.8) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. During the addition, the reaction liquid temperature is maintained at 100°C.

[0107] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 110°C and the reaction is carried out for 4 hours.

[0108] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0109] The yield of the above-mentioned combined product is 1.22% and the purity is 97.51%.

[0110] That is, the difference between this comparative example and Example 4 is that the dropping temperature and the reaction temperature are different.

[0111] Comparative Example 4 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0112] S2: After the water removal is completed, the temperature is raised to 110°C, and 120 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:0.8) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. During the addition, the reaction liquid temperature is maintained at 100°C.

[0113] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 115°C and the reaction is carried out for 4 hours.

[0114] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0115] The yield of the above-mentioned combined product is 7.70% and the purity is 98.91%.

[0116] That is, the difference between this comparative example and Example 4 is that the dropping temperature and the reaction temperature are different.

[0117] Comparative Example 5 S1: Add 246.5 g of cumene into a four-necked flask, insert a thermometer, connect a straight condenser to the thorn-shaped distillation column, turn on mechanical stirring, set the oil bath temperature to 105°C, and remove water for 0.5 h.

[0118] S2: After the water is removed, the temperature is raised to 120°C, and 120 g of di-tert-butyl peroxide (the molar ratio of cumene to di-tert-butyl peroxide is 2:0.8) is slowly added dropwise using a constant pressure dropping funnel at a dropping speed of 1 s / drop. During the addition, the reaction liquid temperature is maintained at 110°C.

[0119] S3: After all the di-tert-butyl peroxide has been dripped, the temperature is raised to 130°C and the reaction is carried out for 4 hours.

[0120] S4: After the reaction is completed, the flask is placed at room temperature and stirred. After the temperature of the reaction liquid drops, crystallization is carried out and the solid obtained after the first filtration is added to 100 mL of methanol and stirred for 1 hour. The solid obtained after the second filtration is dried to obtain the product Lianku.

[0121] The yield of the above-mentioned combined product is 13.34% and the purity is 98.02%.

[0122] That is, the difference between this comparative example and Example 4 is that the dropping temperature and the reaction temperature are different.

[0123] Test example The yield and purity of the co-deoxyribonucleic acid obtained in the above Examples 1 to 7 and Comparative Examples 1 to 5 were compared, and the results are shown in Tables 1 to 3.

[0124] Table 1 Comparison results

[0125] It can be seen from Table 1 that the co-dried product prepared by the method provided by the present invention can obtain a co-dried product with higher purity under the conditions of lower cost and simple process.

[0126] Among them, the differences between Example 4 and Comparative Examples 1 and 2 in Table 1 and the corresponding effects are more intuitively listed as shown in Table 2.

[0127] Table 2 Comparison results

[0128] Table 2 shows that different ways of adding di-tert-butyl peroxide will lead to significant differences in the yield of co-condensation.

[0129] In addition, the differences between Example 4 and Comparative Examples 3 to 5 in Table 1 and the corresponding effects are more intuitively listed as shown in Table 3.

[0130] Table 3 Comparison results

[0131] It can be proved from Table 3 that different dropping temperatures and reaction temperatures will also lead to significant differences in the co-depletion yield.

[0132] In summary, the preparation method of the co-cured oil provided by the present invention is simple to operate, low in cost, requires only one initiator, has a short reaction time, generates no wastewater, is environmentally friendly, and can obtain co-cured oil with high purity. The obtained co-cured oil can be used for flame retardant enhancement, polymer modification, or initiation of high-temperature polymer reactions, etc.

[0133] 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 a linalool, characterized in that: The following steps are involved: Adding di-tert-butyl peroxide to cumene at a temperature of ≥130° C. and <140° C. for reaction; The molar ratio of the isopropylbenzene to the di-tert-butyl peroxide is 2:0.6 to 2:1.4, the addition rate of the di-tert-butyl peroxide is 1 s / drop to 2 s / drop, the reaction temperature does not exceed 150° C., and the reaction time is not less than 4 hours.

2. The preparation method according to claim 1, characterized in that: Heat cumene to a temperature ≥100°C and <140°C using an oil bath.

3. The preparation method according to claim 2, characterized in that: The isopropylbenzene heated in an oil bath to ≥100°C and <140°C is first subjected to a dehydration treatment, the temperature of the dehydrated isopropylbenzene is controlled to be ≥130°C and <140°C, and then the di-tert-butyl peroxide is added.

4. The preparation method according to any one of claims 1 to 3, characterized in that Reaction temperature ≥135°C and <150°C; Preferably, the reaction temperature is 140°C to 145°C.

5. The preparation method according to claim 4, characterized in that: During the addition of di-tert-butyl peroxide, the temperature of the reaction solution was maintained at not less than 125°C.

6. The preparation method according to claim 4, characterized in that: The reaction time is 4h~6h.

7. The preparation method according to claim 1, characterized in that: Also includes: After the reaction is completed, the reaction liquid is crystallized to separate the solid and the liquid to obtain a solid; Preferably, the method further comprises: washing and drying the solid.

8. The preparation method according to claim 1, characterized in that: Also includes: The liquid obtained by solid-liquid separation is used as the raw material for the next synthesis of dry products; Preferably, the method further comprises: fractionating the distillate in the reaction process to obtain fractions, and recycling the fractions.

9. A joint dry, characterized in that, Prepared by the preparation method according to any one of claims 1 to 8; Preferably, the joint has at least one of the following characteristics: Feature 1: The yield of the linked dry product is not less than 16%; Feature 2: The purity of the deionized water is not less than 96%.

10. A use of the joint dry as claimed in claim 9, characterized in that: The dimethicone is used for flame retardant enhancement, polymer modification or initiation of high temperature polymer reaction.

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