Production device and method of ethylhexylglycerin
By using simple equipment and low-investment production equipment in the synthesis process of ethylhexylglycerol, combining cyclization reaction and hydrolysis reaction, and using Lewis acid catalyst, the problems of large catalyst usage and harsh reaction conditions in the prior art are solved, and the reaction conditions are harsh, thus achieving the following: Efficient and economical synthesis of ethylhexylglycerol.
Patent Information
- Application Number
- CN202411562778.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-05
- Publication Date
- 2025-02-14
AI Technical Summary
The existing ethylhexylglycerol synthesis methods have problems such as large amount of catalyst usage, harsh reaction conditions, high catalyst cost, and large amounts of wastewater generated during the reaction.
Using a simple equipment structure and a low-investment production device, the reaction is carried out by combining cyclization reaction and hydrolysis reaction, and the reaction conditions are controlled to reduce wastewater generation.
It has achieved efficient synthesis of ethylhexylglycerol, low catalyst usage, economical cost, mild reaction conditions, less wastewater and high production efficiency.
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Figure CN119431123A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of preservative processing, and in particular relates to a production device and method for ethylhexylglycerin. Background Art
[0002] Ethylhexylglycerol (EHG), also known as 2-ethylhexylglycerol, is an important organic compound. EHG has certain bactericidal ability and moisturizing and wetting functions, and does not irritate the skin, so it is widely used as a preservative in daily chemical products.
[0003] In industrial production, there are many methods for synthesizing ethylhexylglycerol, among which the most common method is chemical synthesis. Chemical synthesis methods mainly include inorganic acid catalytic synthesis, inorganic base catalytic synthesis and enzyme catalytic synthesis. Although these methods can achieve the synthesis of ethylhexylglycerol, there are some problems, such as large amount of catalyst used, harsh reaction conditions, high catalyst cost, and large amount of wastewater generated during the reaction.
[0004] In view of this, the present invention provides a production device and method for ethylhexylglycerol. The equipment structure of the present invention is simple and the investment is low; the ethylhexylglycerol synthesis method of the present invention has the advantages of mild reaction conditions, low catalyst cost, less waste water, high production efficiency, etc.
[0005] The present invention mainly involves two reactions, such as Figure 3 As shown, there is a cyclization reaction and a hydrolysis reaction.
[0006] Cyclization reaction: Ethylhexyl glyceryl ether (hereinafter referred to as glyceryl ether) and acetone undergo cyclization reaction in the presence of a catalyst to generate 4-alkoxymethyl-1,3-dioxolane (hereinafter referred to as dioxolane).
[0007] Hydrolysis reaction: Dioxolane reacts with water under certain conditions to produce ethylhexylglycerin. Summary of the invention
[0008] In order to make up for the deficiencies of the prior art and solve the above technical problems, the present invention proposes a production device and method for ethylhexylglycerol. The equipment structure of the present invention is simple and the investment is low. The ethylhexylglycerol synthesis method of the present invention has the advantages of mild reaction conditions, low catalyst cost, less waste water, high production efficiency, etc. The specifics are as follows:
[0009] A method for producing ethylhexylglycerin comprises the following steps:
[0010] S1: adding acetone, glycerol ether and catalyst into a reactor in a mass ratio of 0.9-3.1:1:0.002-0.01 to carry out a cyclization reaction, controlling the cyclization reaction temperature at 10-40° C. and stirring the reaction for 3-12 hours;
[0011] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride or boron trifluoride etherate;
[0012] S2: After the cyclization reaction is completed, water is added to the reactor, and a hydrolysis reaction is carried out at 55-85°C, and the reaction is stirred for 4-12 hours;
[0013] The amount of water added is 20% to 90% of the mass of the glycerol ether feed;
[0014] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 30-40°C;
[0015] S3: After the hydrolysis is completed, the material temperature is raised to 90-95°C, and the acetone is evaporated to obtain a crude ethylhexylglycerol;
[0016] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0017] S4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing under the condition that the water washing kettle is stirred and turned on;
[0018] The water washing times are 1 to 3 times, each time the water washing is stirred for 0.5 to 1 hour, and then it is left to stand for 2 to 4 hours, the mixed material is divided into two layers of oil and water, the oil phase is on the upper side, and the water phase is on the lower side, and the catalyst is extracted into the water;
[0019] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5 to 2:1;
[0020] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0021] The pH of the oil phase after water washing is 5-7; the oil phase after water washing is input into the material buffer tank;
[0022] S5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0023] Wherein, the pressure of the EHG side sampling port is 10-50 Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 100-125° C.;
[0024] Wherein, the temperature of the material after condensation in the tower condenser is 10-40°C.
[0025] Specifically, a method for producing ethylhexylglycerin comprises the following specific steps:
[0026] A1: Add acetone, glycerol ether and catalyst into a reactor in a mass ratio of 0.9:1:0.002 to carry out cyclization reaction. The cyclization reaction temperature is controlled at 10°C and the reaction is stirred for 12 hours.
[0027] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride;
[0028] A2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 55°C, and the reaction is stirred for 12 hours;
[0029] The amount of water added is 20% of the mass of the glycerol ether feed;
[0030] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 30°C;
[0031] A3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0032] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0033] A4: The crude ethylhexylglycerol product is transported to a water washing kettle, and a certain proportion of water is added to the crude ethylhexylglycerol product from the reaction kettle for water washing while stirring the water washing kettle;
[0034] The water washing times were 1, each time the water washing was stirred for 1 hour, and then left to stand for 4 hours, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0035] Wherein, the mass ratio of water to crude ethylhexylglycerin is 2:1;
[0036] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0037] The pH of the oil phase after water washing is 5.1; the oil phase after water washing is input into the material buffer tank;
[0038] A5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0039] Wherein, the pressure of the EHG side sampling port is 10Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 100°C;
[0040] Wherein, the temperature of the material after condensation in the tower condenser is 10°C;
[0041] Wherein, the distillation tower is a molecular distillation device.
[0042] Specifically, a method for producing ethylhexylglycerin comprises the following specific steps:
[0043] B1: Acetone, glycerol ether and catalyst were added into a reactor in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 20°C and stirred for 9 hours.
[0044] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride;
[0045] B2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 65°C and stirred for 8 hours;
[0046] The amount of water added is 40% of the mass of the glycerol ether feed;
[0047] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 35°C;
[0048] B3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0049] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0050] B4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle;
[0051] The water washing times were 2 times, each time the water washing was stirred for 1 hour, and then left to stand for 3 hours, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0052] Wherein, the mass ratio of water to crude ethylhexylglycerin is 1:1;
[0053] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0054] The pH of the oil phase after water washing is 6.2; the oil phase after water washing is input into the material buffer tank;
[0055] B5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0056] Wherein, the pressure of the EHG side sampling port is 20Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 110°C;
[0057] Wherein, the temperature of the material after condensation in the tower condenser is 20°C;
[0058] Wherein, the distillation tower is a molecular distillation device.
[0059] Specifically, a method for producing ethylhexylglycerin comprises the following specific steps:
[0060] C1: Acetone, glycerol ether and catalyst were added into a reactor in a mass ratio of 2:1:0.008 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours.
[0061] Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate;
[0062] C2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 75°C and stirred for 6 hours;
[0063] The amount of water added is 60% of the mass of the glycerol ether feed;
[0064] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 40°C;
[0065] C3: After the hydrolysis is completed, the material temperature is raised to 95°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0066] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0067] C4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing under the condition that the water washing kettle is stirred and turned on;
[0068] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0069] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0070] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0071] The pH of the oil phase after water washing is 6.7; the oil phase after water washing is input into the material buffer tank;
[0072] C5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0073] Wherein, the pressure of the EHG side sampling port is 30Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 115°C;
[0074] Wherein, the temperature of the material after condensation in the tower condenser is 30°C;
[0075] Wherein, the distillation tower is a molecular distillation device.
[0076] Specifically, a method for producing ethylhexylglycerin comprises the following specific steps:
[0077] D1: Acetone, glycerol ether and catalyst were added into the reactor in a mass ratio of 3.1:1:0.01 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 40°C and stirred for 3 hours.
[0078] Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate;
[0079] D2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 85°C and stirred for 4 hours;
[0080] The amount of water added is 90% of the mass of the glycerol ether feed;
[0081] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 30°C;
[0082] D3: After the hydrolysis is completed, the material temperature is raised to 95°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0083] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0084] D4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle;
[0085] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0086] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0087] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0088] The pH of the oil phase after water washing is 6.5; the oil phase after water washing is input into the material buffer tank;
[0089] D5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0090] Wherein, the pressure of the EHG side sampling port is 40Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 120°C;
[0091] Wherein, the temperature of the material after condensation in the tower condenser is 40°C;
[0092] Wherein, the distillation tower is a packed tower.
[0093] Specifically, a method for producing ethylhexylglycerin comprises the following specific steps:
[0094] E1: Acetone, glycerol ether and catalyst were added into the reactor in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours.
[0095] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride;
[0096] E2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 75°C and stirred for 6 hours;
[0097] The amount of water added is 60% of the mass of the glycerol ether feed;
[0098] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 40°C;
[0099] E3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0100] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0101] E4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle;
[0102] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0103] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0104] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0105] The pH of the oil phase after water washing is 6.8; the oil phase after water washing is input into the material buffer tank;
[0106] E5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0107] Wherein, the pressure of the EHG side sampling port is 50Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 125°C;
[0108] Wherein, the temperature of the material after condensation in the tower condenser is 30°C;
[0109] Wherein, the distillation tower is a packed tower.
[0110] Specifically, a method for producing ethylhexylglycerin comprises the following specific steps:
[0111] F1: Acetone, glycerol ether and catalyst were added into the reactor in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours.
[0112] Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate;
[0113] F2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 75°C and stirred for 6 hours;
[0114] The amount of water added is 60% of the mass of the glycerol ether feed;
[0115] During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 40°C;
[0116] F3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0117] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0118] F4: transporting the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle;
[0119] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0120] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0121] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0122] The pH of the oil phase after water washing is 6.5; the oil phase after water washing is input into the material buffer tank;
[0123] F5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port;
[0124] Wherein, the pressure of the EHG side sampling port is 30Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 115°C;
[0125] Wherein, the distillation tower is a plate tower.
[0126] An ethylhexylglycerol production device, suitable for the above-mentioned ethylhexylglycerol production method, comprising a reaction kettle, a reaction condenser, a water washing kettle, a material buffer tank and a distillation system;
[0127] Wherein, the distillation system comprises a distillation tower, a tower condenser, a reflux tank and a reboiler;
[0128] The inlet materials of the reactor are ethylhexyl glycidyl ether, acetone, catalyst and water;
[0129] The discharge port of the reaction kettle is connected to an inlet of the water washing kettle;
[0130] The reactor is provided with a stirrer and a reaction condenser, and the reactor is provided with a half pipe or a jacket for cooling or heating;
[0131] The upper part of the water washing kettle is provided with a second water inlet, and the bottom is provided with a water phase outlet and an oil phase inlet. The water phase outlet is provided with an online conductivity monitoring system, and the conductivity is interlocked with the cut-off valves of the oil phase outlet and the water phase outlet;
[0132] The oil phase discharge port of the water washing kettle is connected to the distillation tower through the material buffer tank, and the wastewater at the water phase outlet is transported to the subsequent process section for treatment;
[0133] The water washing kettle is provided with a stirrer and a heating half pipe or a jacket;
[0134] The distillation tower is a packed tower, a plate tower, or a molecular distillation device.
[0135] The beneficial effects of the present invention are as follows:
[0136] (1) The equipment of the present invention has a simple structure, low investment, and is easy to operate, which is conducive to industrial promotion.
[0137] (2) The cyclization reaction of the present invention uses a catalyst in an amount of less than 1%, which is low in cost, mild in reaction conditions, and low in energy consumption.
[0138] (3) The hydrolysis reaction of the present invention does not require the addition of a catalyst, and the catalyst for the cyclization reaction does not need to be "quenched", resulting in a small amount of wastewater.
[0139] (4) The process of the present invention is simple, the cyclization reaction and the hydrolysis reaction are carried out in the same reactor, the equipment utilization rate is high, the loss of raw materials is small, and the total yield of ethylhexylglycerol is greater than 90%. BRIEF DESCRIPTION OF THE DRAWINGS
[0140] The present invention will be further described below in conjunction with the accompanying drawings.
[0141] Figure 1 This is a schematic diagram of the ethylhexylglycerin production device of the present invention;
[0142] Figure 2 is a graph showing the relationship between the boiling point and pressure of ethylhexylglycerol in the present invention;
[0143] Figure 3 It is a schematic diagram of the cyclization reaction and the hydrolysis reaction in the present invention;
[0144] In the figure: 1. Reactor; 2. Reaction condenser; 3. Water washing kettle; 4. Material buffer tank; 5. Distillation tower; 6. Tower condenser; 7. Reflux tank; 8. Reboiler. DETAILED DESCRIPTION
[0145] In order to make the technical means, creative features, objectives and effects achieved by the present invention easy to understand, the present invention is further explained below in conjunction with specific implementation methods.
[0146] Example 1: Figures 1 to 3 As shown, on the one hand, the present invention provides a method for producing ethylhexylglycerol, comprising the following steps:
[0147] S1: adding acetone, glycerol ether and catalyst into reactor 1 in a mass ratio of 0.9-3.1:1:0.002-0.01 to carry out cyclization reaction, controlling the cyclization reaction temperature at 10-40° C., and stirring the reaction for 3-12 hours;
[0148] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride or boron trifluoride etherate;
[0149] S2: After the cyclization reaction is completed, water is added to the reactor 1, and a hydrolysis reaction is carried out at 55-85°C, and the reaction is stirred for 4-12 hours;
[0150] The amount of water added is 20% to 90% of the mass of the glycerol ether feed;
[0151] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the material after condensation is 30-40°C;
[0152] S3: After the hydrolysis is completed, the material temperature is raised to 90-95°C, and the acetone is evaporated to obtain a crude ethylhexylglycerol;
[0153] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0154] S4: conveying the crude ethylhexylglycerol to the water washing kettle 3, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle 1 for water washing under the condition that the water washing kettle 3 is stirred and turned on;
[0155] The water washing times are 1 to 3 times, each time the water washing is stirred for 0.5 to 1 hour, and then it is left to stand for 2 to 4 hours, the mixed material is divided into two layers of oil and water, the oil phase is on the upper side, and the water phase is on the lower side, and the catalyst is extracted into the water;
[0156] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5 to 2:1;
[0157] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0158] The pH of the oil phase after water washing is 5-7; the oil phase after water washing is input into the material buffer tank 4;
[0159] S5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0160] Wherein, the pressure of the EHG side sampling port is 10-50 Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 100-125° C.;
[0161] The temperature of the material after condensation in the tower condenser 6 is 10-40°C.
[0162] Example 2: Based on Example 1, the present invention provides a method for producing ethylhexylglycerol, which, when used, specifically comprises the following steps:
[0163] A1: Add acetone, glycerol ether and catalyst in a mass ratio of 0.9:1:0.002 into reactor 1 to carry out cyclization reaction. The cyclization reaction temperature is controlled at 10°C and the reaction is stirred for 12 hours.
[0164] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride;
[0165] A2: After the cyclization reaction is completed, water is added to the reactor 1, and a hydrolysis reaction is carried out at 55°C, and the reaction is stirred for 12 hours;
[0166] The amount of water added is 20% of the mass of the glycerol ether feed;
[0167] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the material after condensation is 30°C;
[0168] A3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0169] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0170] A4: The crude ethylhexylglycerol product is transported to the water washing kettle 3. Under the condition that the water washing kettle 3 is stirred and turned on, a certain proportion of water is added to the crude ethylhexylglycerol product from the reaction kettle 1 for water washing;
[0171] The water washing times were 1, each time the water washing was stirred for 1 hour, and then left to stand for 4 hours, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0172] Wherein, the mass ratio of water to crude ethylhexylglycerin is 2:1;
[0173] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0174] The pH of the oil phase after water washing is 5.1; the oil phase after water washing is input into the material buffer tank 4;
[0175] A5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0176] Wherein, the pressure of the EHG side sampling port is 10Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 100°C;
[0177] The temperature of the material after condensation in the tower condenser 6 is 10°C.
[0178] Wherein, the distillation tower 5 is a molecular distillation device.
[0179] According to the production method of ethylhexylglycerol described in Example 2, the total yield of ethylhexylglycerol obtained is 92.8%, and the purity of ethylhexylglycerol is 99.32%.
[0180] Example 3: Based on Example 1, the production method of ethylhexylglycerol provided by the present invention, when used, specifically comprises the following steps:
[0181] B1: Acetone, glycerol ether and catalyst were added into reactor 1 in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 20° C. and stirred for 9 hours.
[0182] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride;
[0183] B2: After the cyclization reaction is completed, water is added to the reactor 1, and a hydrolysis reaction is carried out at 65°C, and the reaction is stirred for 8 hours;
[0184] The amount of water added is 40% of the mass of the glycerol ether feed;
[0185] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the condensed material is 35°C;
[0186] B3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0187] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0188] B4: transporting the crude ethylhexylglycerol to the water washing kettle 3, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle 1 for water washing under the condition that the water washing kettle 3 is stirred and turned on;
[0189] The water washing times were 2 times, each time the water washing was stirred for 1 hour, and then left to stand for 3 hours, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0190] Wherein, the mass ratio of water to crude ethylhexylglycerin is 1:1;
[0191] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0192] The pH of the oil phase after water washing is 6.2; the oil phase after water washing is input into the material buffer tank 4;
[0193] B5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0194] Wherein, the pressure of the EHG side sampling port is 20Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 110°C;
[0195] The temperature of the material after condensation in the tower condenser 6 is 20°C.
[0196] Wherein, the distillation tower 5 is a molecular distillation device.
[0197] According to the production method of ethylhexylglycerol described in Example 3, the total yield of ethylhexylglycerol obtained is 94.5%, and the purity of ethylhexylglycerol is 99.53%.
[0198] Example 4: Based on Example 1, the production method of ethylhexylglycerol provided by the present invention, when used, specifically comprises the following steps:
[0199] C1: Acetone, glycerol ether and catalyst were added into reactor 1 in a mass ratio of 2:1:0.008 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30° C. and stirred for 6 hours.
[0200] Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate;
[0201] C2: After the cyclization reaction is completed, water is added to the reactor 1, and the hydrolysis reaction is carried out at 75°C, and the reaction is stirred for 6 hours;
[0202] The amount of water added is 60% of the mass of the glycerol ether feed;
[0203] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the condensed material is 40°C;
[0204] C3: After the hydrolysis is completed, the material temperature is raised to 95°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0205] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0206] C4: conveying the crude ethylhexylglycerol to the water washing kettle 3, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle 1 for water washing under the condition that the water washing kettle 3 is stirred and turned on;
[0207] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0208] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0209] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0210] The pH of the oil phase after water washing is 6.7; the oil phase after water washing is input into the material buffer tank 4;
[0211] C5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0212] Wherein, the pressure of the EHG side sampling port is 30Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 115°C;
[0213] The temperature of the material after condensation in the tower condenser 6 is 30°C.
[0214] The distillation tower 5 is a molecular distillation device.
[0215] According to the production method of ethylhexylglycerol described in Example 4, the total yield of ethylhexylglycerol obtained is 94.9%, and the purity of ethylhexylglycerol is 99.71%.
[0216] Example 5: Based on Example 1, the production method of ethylhexylglycerol provided by the present invention, when used, specifically comprises the following steps:
[0217] D1: Acetone, glycerol ether and catalyst were added into reactor 1 in a mass ratio of 3.1:1:0.01 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 40°C and stirred for 3 hours.
[0218] Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate;
[0219] D2: After the cyclization reaction is completed, water is added to the reactor 1, and the hydrolysis reaction is carried out at 85°C, and the reaction is stirred for 4 hours;
[0220] The amount of water added is 90% of the mass of the glycerol ether feed;
[0221] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the material after condensation is 30°C;
[0222] D3: After the hydrolysis is completed, the material temperature is raised to 95°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0223] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0224] D4: The crude ethylhexylglycerol product is transported to the water washing kettle 3. Under the condition that the water washing kettle 3 is stirred and turned on, a certain proportion of water is added to the crude ethylhexylglycerol product from the reaction kettle 1 for water washing;
[0225] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0226] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0227] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0228] The pH of the oil phase after water washing is 6.5; the oil phase after water washing is input into the material buffer tank 4;
[0229] D5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0230] Wherein, the pressure of the EHG side sampling port is 40Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 120°C;
[0231] The temperature of the material after condensation in the tower condenser 6 is 40°C.
[0232] Wherein, the distillation tower 5 is a packed tower.
[0233] Among them, according to the production method of ethylhexylglycerol described in Example 5, the total yield of ethylhexylglycerol obtained is 90.1%, and the purity of ethylhexylglycerol is 99.14%.
[0234] Example 6: Based on Example 1, the production method of ethylhexylglycerol provided by the present invention, when used, specifically comprises the following steps:
[0235] E1: Acetone, glycerol ether and catalyst were added into reactor 1 in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours.
[0236] Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride;
[0237] E2: After the cyclization reaction is completed, water is added to the reactor 1, and the hydrolysis reaction is carried out at 75°C, and the reaction is stirred for 6 hours;
[0238] The amount of water added is 60% of the mass of the glycerol ether feed;
[0239] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the condensed material is 40°C;
[0240] E3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0241] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0242] E4: transporting the crude ethylhexylglycerol to the water washing kettle 3, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle 1 for water washing under the condition that the water washing kettle 3 is stirred and turned on;
[0243] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0244] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0245] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0246] The pH of the oil phase after water washing is 6.8; the oil phase after water washing is input into the material buffer tank 4;
[0247] E5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0248] Wherein, the pressure of the EHG side sampling port is 50Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 125°C;
[0249] The temperature of the material after condensation in the tower condenser 6 is 30°C.
[0250] The distillation tower 5 is a molecular distillation device.
[0251] Among them, according to the production method of ethylhexylglycerol described in Example 6, the total yield of ethylhexylglycerol obtained is 92.3%, and the purity of ethylhexylglycerol is 99.38%.
[0252] Example 7: Based on Example 1, the production method of ethylhexylglycerol provided by the present invention, when used, specifically comprises the following steps:
[0253] F1: Acetone, glycerol ether and catalyst were added into reactor 1 in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours.
[0254] Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate;
[0255] F2: After the cyclization reaction, water was added to the reactor 1, and the hydrolysis reaction was carried out at 75°C, and the reaction was stirred for 6 hours;
[0256] The amount of water added is 60% of the mass of the glycerol ether feed;
[0257] During the hydrolysis process, the reaction condenser 2 needs to be opened, and the temperature of the condensed material is 40°C;
[0258] F3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol;
[0259] The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration;
[0260] F4: transporting the crude ethylhexylglycerol to the water washing kettle 3, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle 1 for water washing under the condition that the water washing kettle 3 is stirred and turned on;
[0261] The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water;
[0262] Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1;
[0263] Wherein, the water phase is transported to the subsequent wastewater section for treatment;
[0264] The pH of the oil phase after water washing is 6.5; the oil phase after water washing is input into the material buffer tank 4;
[0265] F5: The oil phase material from the material buffer tank 4 is subjected to vacuum distillation in the distillation tower 5, and the ethylhexylglycerol product is produced through the EHG side production port;
[0266] Wherein, the pressure of the EHG side sampling port is 30Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 115°C;
[0267] The temperature of the material after condensation in the tower condenser 6 is 30°C.
[0268] Among them, according to the production method of ethylhexylglycerol described in Example 7, the total yield of ethylhexylglycerol obtained is 93.6%, and the purity of ethylhexylglycerol is 99.45%.
[0269] Wherein, the distillation tower 5 is a plate tower.
[0270] It should be noted that, during the implementation of Examples 1 to 7, since ethylhexyl glycerol has a relatively high boiling point, which is about 300° C. under normal pressure, in order to avoid oxidation and deterioration of ethylhexyl glycerol during the refining process, it is necessary to perform vacuum distillation on the crude ethylhexyl glycerol. Through testing, a boiling point-pressure relationship diagram of ethylhexyl glycerol can be obtained, as shown in FIG. Figure 2 As shown, if the extraction temperature of ethylhexylglycerol is controlled below 145°C, the pressure of the system should be less than 200Pa.
[0271] On the other hand, the present invention also provides an ethylhexylglycerol production device, comprising a reaction kettle 1, a reaction condenser 2, a water washing kettle 3, a material buffer tank 4 and a distillation system;
[0272] Wherein, the distillation system comprises a distillation tower 5, a tower condenser 6, a reflux tank 7 and a reboiler 8;
[0273] The inlet materials of reactor 1 are ethylhexyl glycidyl ether, acetone, catalyst and water;
[0274] The discharge port of the reaction kettle 1 is connected to an inlet of the water washing kettle 3;
[0275] The reactor 1 is provided with a stirrer and a reaction condenser 2. The reactor 1 is provided with a half pipe or a jacket for cooling or heating;
[0276] The upper part of the water washing kettle 3 is provided with a second water inlet, and the bottom is provided with a water phase outlet and an oil phase inlet. The water phase outlet is provided with an online conductivity monitoring system, and the conductivity is interlocked with the cut-off valves of the oil phase outlet and the water phase outlet;
[0277] The oil phase discharge port of the water washing kettle 3 is connected to the distillation tower 5 through the material buffer tank 4, and the waste water at the water phase outlet is transported to the subsequent process section for treatment;
[0278] The water washing kettle 3 is provided with a stirrer and a heating half pipe or a jacket;
[0279] The distillation tower 5 is a packed tower, a plate tower, or a molecular distillation device.
[0280] It should be noted that, in the actual operation process of the ethylhexylglycerol production device provided by the present invention, Figure 1 As shown, ethylhexyl glycidyl ether enters from the glycidyl ether inlet A, acetone enters from the acetone inlet B, the catalyst enters from the catalyst inlet, and water enters from the first water inlet D into the reactor 1;
[0281] Further, water enters the water washing kettle 3 from the second water inlet E, crude acetone is discharged from the crude acetone outlet F, and waste water is discharged from the waste water outlet G;
[0282] Furthermore, ethylhexylglycerol is discharged from the EHG side outlet, I is the light component outlet, and J is the tower bottom residual liquid outlet.
[0283] The above shows and describes the basic principles, main features and advantages of the present invention. It should be understood by those skilled in the art that the present invention is not limited to the above embodiments. The above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, which fall within the scope of the present invention. The scope of protection of the present invention is defined by the attached claims and their equivalents.
Claims
1. A method for producing ethylhexylglycerol, characterized in that: The steps include: S1: adding acetone, glycerol ether and catalyst into a reactor in a mass ratio of 0.9-3.1:1:0.002-0.01 to carry out a cyclization reaction, controlling the cyclization reaction temperature at 10-40° C. and stirring the reaction for 3-12 hours; Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride or boron trifluoride etherate; S2: After the cyclization reaction is completed, water is added to the reactor, and a hydrolysis reaction is carried out at 55-85°C, and the reaction is stirred for 4-12 hours; The amount of water added is 20% to 90% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 30-40°C; S3: After the hydrolysis is completed, the material temperature is raised to 90-95°C, and the acetone is evaporated to obtain a crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; S4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing under the condition that the water washing kettle is stirred and turned on; The water washing times are 1 to 3 times, each time the water washing is stirred for 0.5 to 1 hour, and then it is left to stand for 2 to 4 hours, the mixed material is divided into two layers of oil and water, the oil phase is on the upper side, and the water phase is on the lower side, and the catalyst is extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5 to 2:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 5-7; the oil phase after water washing is input into the material buffer tank; S5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 10-50 Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 100-125° C.; Wherein, the temperature of the material after condensation in the tower condenser is 10-40°C.
2. The method for producing ethylhexylglycerol according to claim 1, characterized in that: The steps include: A1: Add acetone, glycerol ether and catalyst into a reactor in a mass ratio of 0.9:1:0.002 to carry out cyclization reaction. The cyclization reaction temperature is controlled at 10°C and the reaction is stirred for 12 hours. Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride; A2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 55°C, and the reaction is stirred for 12 hours; The amount of water added is 20% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 30°C; A3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; A4: The crude ethylhexylglycerol product is transported to a water washing kettle, and a certain proportion of water is added to the crude ethylhexylglycerol product from the reaction kettle for water washing while stirring the water washing kettle; The water washing times were 1, each time the water washing was stirred for 1 hour, and then left to stand for 4 hours, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 2:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 5.1; the oil phase after water washing is input into the material buffer tank; A5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 10Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 100°C; Wherein, the temperature of the material after condensation in the tower condenser is 10°C; Wherein, the distillation tower is a molecular distillation device.
3. The method for producing ethylhexylglycerol according to claim 1, characterized in that: The steps include: B1: Acetone, glycerol ether and catalyst were added into a reactor in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 20°C and stirred for 9 hours. Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride; B2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 65°C and stirred for 8 hours; The amount of water added is 40% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 35°C; B3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; B4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle; The water washing times were 2 times, each time the water washing was stirred for 1 hour, and then it was left to stand for 3 hours, the mixed material was divided into two layers of oil and water, the oil phase was on the upper side, and the water phase was on the lower side, and the catalyst was extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 1:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 6.2; the oil phase after water washing is input into the material buffer tank; B5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 20Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 110°C; Wherein, the temperature of the material after condensation in the tower condenser is 20°C; Wherein, the distillation tower is a molecular distillation device.
4. The method for producing ethylhexylglycerol according to claim 1, characterized in that: The steps include: C1: Acetone, glycerol ether and catalyst were added into a reactor in a mass ratio of 2:1:0.008 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours. Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate; C2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 75°C and stirred for 6 hours; The amount of water added is 60% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 40°C; C3: After the hydrolysis is completed, the material temperature is raised to 95°C, and the acetone is evaporated to obtain crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; C4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing under the condition that the water washing kettle is stirred and turned on; The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 6.7; the oil phase after water washing is input into the material buffer tank; C5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 30Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 115°C; Wherein, the temperature of the material after condensation in the tower condenser is 30°C; Wherein, the distillation tower is a molecular distillation device.
5. The method for producing ethylhexylglycerol according to claim 1, characterized in that: The steps include: D1: Acetone, glycerol ether and catalyst were added into the reactor in a mass ratio of 3.1:1:0.01 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 40°C and stirred for 3 hours. Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate; D2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 85°C and stirred for 4 hours; The amount of water added is 90% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 30°C; D3: After the hydrolysis is completed, the material temperature is raised to 95°C, and the acetone is evaporated to obtain crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; D4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle; The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 6.5; the oil phase after water washing is input into the material buffer tank; D5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 40Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 120°C; Wherein, the temperature of the material after condensation in the tower condenser is 40°C; Wherein, the distillation tower is a packed tower.
6. The method for producing ethylhexylglycerol according to claim 1, characterized in that: The steps include: E1: Acetone, glycerol ether and catalyst were added into the reactor in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours. Wherein, the catalyst is Lewis acid, and the catalyst is zinc chloride; E2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 75°C and stirred for 6 hours; The amount of water added is 60% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 40°C; E3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; E4: conveying the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle; The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 6.8; the oil phase after water washing is input into the material buffer tank; E5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 50Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 125°C; Wherein, the temperature of the material after condensation in the tower condenser is 30°C; Wherein, the distillation tower is a packed tower.
7. The method for producing ethylhexylglycerol according to claim 1, characterized in that: The steps include: F1: Acetone, glycerol ether and catalyst were added into the reactor in a mass ratio of 1.5:1:0.005 to carry out cyclization reaction. The cyclization reaction temperature was controlled at 30°C and stirred for 6 hours. Wherein, the catalyst is Lewis acid, and the catalyst is boron trifluoride etherate; F2: After the cyclization reaction is completed, water is added to the reactor, and the hydrolysis reaction is carried out at 75°C and stirred for 6 hours; The amount of water added is 60% of the mass of the glycerol ether feed; During the hydrolysis process, the reaction condenser needs to be turned on, and the temperature of the condensed material is 40°C; F3: After the hydrolysis is completed, the material temperature is raised to 90°C, and the acetone is evaporated to obtain crude ethylhexylglycerol; The evaporated acetone can be recycled after being transported to the subsequent process section for dehydration; F4: transporting the crude ethylhexylglycerol to a water washing kettle, and adding a certain proportion of water to the crude ethylhexylglycerol from the reaction kettle for water washing while stirring the water washing kettle; The water washing times were 3 times, each time the water washing was stirred for 0.5 h, and then left to stand for 2 h, the mixed material was divided into two layers of oil and water, with the oil phase on the upper side and the water phase on the lower side, and the catalyst was extracted into the water; Wherein, the mass ratio of water to crude ethylhexylglycerin is 0.5:1; Wherein, the water phase is transported to the subsequent wastewater section for treatment; The pH of the oil phase after water washing is 6.5; the oil phase after water washing is input into the material buffer tank; F5: The oil phase material from the material buffer tank is subjected to vacuum distillation in a distillation tower, and the ethylhexylglycerol product is produced through the EHG side production port; Wherein, the pressure of the EHG side sampling port is 30Pa, and the temperature of the ethylhexylglycerol at the EHG side sampling port is 115°C; Wherein, the distillation tower is a plate tower.
8. An ethylhexylglycerol production device, suitable for the ethylhexylglycerol production device of claim 1, characterized in that: It includes a reactor, a reaction condenser, a water washing kettle, a material buffer tank and a distillation system; Wherein, the distillation system comprises a distillation tower, a tower condenser, a reflux tank and a reboiler; The inlet materials of the reactor are ethylhexyl glycidyl ether, acetone, catalyst and water; The discharge port of the reaction kettle is connected to an inlet of the water washing kettle; The reactor is provided with a stirrer and a reaction condenser, and the reactor is provided with a half pipe or a jacket for cooling or heating; The upper part of the water washing kettle is provided with a second water inlet, and the bottom is provided with a water phase outlet and an oil phase inlet. The water phase outlet is provided with an online conductivity monitoring system, and the conductivity is interlocked with the cut-off valves of the oil phase outlet and the water phase outlet; The oil phase discharge port of the water washing kettle is connected to the distillation tower through the material buffer tank, and the wastewater at the water phase outlet is transported to the subsequent process section for treatment; The water washing kettle is provided with a stirrer and a heating half pipe or a jacket; The distillation tower is a packed tower, a plate tower, or a molecular distillation device.