CN114835593A - Production process of diethanolisopropanolamine - Google Patents
Production process of diethanolisopropanolamine Download PDFInfo
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- CN114835593A CN114835593A CN202210483438.4A CN202210483438A CN114835593A CN 114835593 A CN114835593 A CN 114835593A CN 202210483438 A CN202210483438 A CN 202210483438A CN 114835593 A CN114835593 A CN 114835593A
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Abstract
The application relates to the field of production of diethanol monoisopropanolamine and discloses a production process of diethanol monoisopropanolamine, which comprises the following steps: adding 2-4 ℃ epoxypropane into a reactor, wherein the pressure in the reactor is 0.1-0.12 MPa, adding 28-30 ℃ mixed material, wherein the total mass ratio of diethanolamine to carbon tetrachloride in the mixed material is more than 99wt%, and the mass ratio of diethanolamine to carbon tetrachloride is 1 (0.06-0.2), maintaining the temperature in the reactor at 4-6 ℃, and mixing the epoxypropane and the mixed material until the mixture is uniform to obtain a reaction material; the reaction materials are heated to 30 ℃, the stirring is kept, the temperature is raised to 68-72 ℃, the temperature is maintained, the heat preservation reaction is continued for 2-3 hours, and the crude product of the diethanol monoisopropanolamine is obtained.
Description
Technical Field
The application relates to the field of cement admixture production, in particular to a production process of diethanol monoisopropanolamine.
Background
The diethanol monoisopropanolamine is a chemical raw material and an intermediate product which are widely applied, a large amount of diethanol monoisopropanolamine is used in a cement admixture and a carbon dioxide trapping agent, the requirement on the purity of the diethanol monoisopropanolamine is high in the using process, and the research on the production process of the diethanol monoisopropanolamine from the aspects of process routes, material mixing, product separation and purification and the like is carried out in the industry.
At present, the popular research direction is to produce the product by taking diethanolamine and propylene oxide as raw materials. Taking a reaction kettle as a reactor, adding diethanol amine into propylene oxide with the temperature lower than 10 ℃, mixing the propylene oxide and the diethanol amine, and inhibiting side reaction at low temperature to generate a high-boiling-point side reaction product. And after the diethanol amine is dissolved or uniformly dispersed in the propylene oxide, heating for reaction, so that the reaction positions in the reactor are almost uniformly distributed in the mixed material, the reaction contact is more sufficient, the main reaction rate is high, the side reaction of the propylene oxide is less, and finally the product of the diethanol monopropanolamine is obtained by reduced pressure distillation.
In the experiments of the inventor of the present application for the related art mentioned above, it was found that:
because the melting point of diethanolamine is 28 ℃ under normal pressure, the diethanolamine is mixed with the propylene oxide with the temperature below 10 ℃, the diethanolamine is rapidly cooled and solidified after contacting the propylene oxide, the mixing speed between the diethanolamine and the propylene oxide is slow, meanwhile, external cooling is needed to control the temperature in a reactor in the mixing process, the mixing speed is further restricted, even if the mechanical stirring is provided by the prior industrial technology, the mixing of the diethanolamine and the propylene oxide needs a longer time, and the problem of long actual production period is caused.
Disclosure of Invention
In order to improve the production efficiency of synthesizing diethanol monoisopropanolamine from diethanol amine and propylene oxide, the application provides a production process of diethanol monoisopropanolamine.
The production process of the diethanol monoisopropanolamine adopts the following technical scheme:
a production process of diethanol monoisopropanolamine comprises the following steps:
s1: adding 2-4 ℃ epoxypropane into a reactor, regulating the pressure with inert gas, wherein the pressure in the reactor is 0.1-0.12 MPa, adding a mixed material into the reactor, wherein the temperature of the mixed material is 28-30 ℃, the total mass ratio of diethanol amine to carbon tetrachloride in the mixed material is more than 99wt%, the mass ratio of diethanol amine to carbon tetrachloride in the mixed material is 1 (0.06-0.2), keeping the reactor refrigerated, keeping the temperature in the reactor at 4-6 ℃, and mixing the epoxypropane and the mixed material until the epoxypropane and the mixed material are uniformly mixed to obtain a reaction material;
s2: and heating the reaction materials to 30 ℃, keeping stirring and heating to 68-72 ℃, maintaining the temperature at 68-72 ℃, and continuing to perform heat preservation reaction for 2-3 hours to obtain a crude product of diethanolisopropanolamine.
By adopting the technical scheme:
mixing diethanolamine and carbon tetrachloride into a mixed material, and dissolving the diethanolamine by the carbon tetrachloride in the process of heating the mixed material to 28-30 ℃ to accelerate the melting of the diethanolamine; after the mixed materials are mixed into a liquid mixed material, the carbon tetrachloride reduces the solidifying point of the mixed material and slows down the phenomenon that the mixed material is solidified by contacting with low-temperature propylene oxide;
when the mixed material is mixed with the epoxypropane, the carbon tetrachloride can promote the mutual solubility of the epoxypropane and the diethanol amine, and even when the temperature of the reactor is maintained at 4-6 ℃, the carbon tetrachloride can promote the fast and efficient mixing of the epoxypropane and the diethanol amine, so that the mixing time is obviously shortened, the production period is shortened, and the energy consumption of refrigeration is reduced.
On the other hand, after the mixed material and the propylene oxide are uniformly mixed to obtain a reaction material, the temperature of the reaction material is raised, the main reaction of synthesizing the diethanol monoisopropanolamine from the propylene oxide and the diethanol amine is rapidly generated, the reaction is an exothermic reaction, and the temperature of the reaction material is continuously raised along with the generation of the reaction. In the actual production process, although a cooling device controls the temperature in the reactor, the controlled reaction temperature is actually a result of reflecting the overall temperature in the reactor or the temperatures at a plurality of sites in the reactor, and a local temperature is still too high due to an excessive main reaction at a local site in the reactor, and a side reaction is also accelerated at the local site due to the excessive local temperature. The occurrence of the local overhigh temperature is difficult to prevent, because the concentration of a certain region is enriched, the local reaction is too violent, the concentration is reduced along with the reaction, the reaction is slowed down, the temperature is reduced, and the prior art cannot realize the mixed preparation of single molecules and single molecules at the grade, and the local overhigh reaction inevitably occurs but cannot be expected.
The carbon tetrachloride added in the application is close to the optimal temperature of reaction control under the process pressure of the application, is higher than the optimal temperature of reaction control and is lower than the boiling points of diethanolamine and diethanol monoisopropanolamine, so that the local temperature caused by over-intense local reaction is too high, the heat energy in a carbon tetrachloride rapid absorption area in the area is used as latent heat, the liquid state is converted into a gaseous state with the same temperature, the reaction heat generated by the diethanol monoisopropanolamine is transferred, the continuous over-intense local reaction is inhibited, the occurrence of over-intense local temperature is reduced, the generation of side reactions is reduced, and the product purity and the yield are improved.
Further optionally, the method further comprises:
s3: purifying the crude product of the diethanol monoisopropanolamine through a purification step including rectification under reduced pressure to obtain a diethanol monoisopropanolamine product; the reduced pressure distillation comprises light component separation for separating carbon tetrachloride and other light components and fine separation for separating diethanolamine.
By adopting the technical scheme, the separation of carbon tetrachloride and other light components and the separation of diethanol amine are divided into two steps for the vacuum distillation purification of the crude diethanol monoisopropanolamine, so that the equipment requirement is reduced, the simultaneous separation of the light components, the carbon tetrachloride, the diethanol amine and the diethanol monoisopropanolamine in a single rectifying tower/rectifying column is avoided, the inappropriate and unreasonable equipment design requirements of a giant rectifying tower (the diameter is more than 5m) or a thin and high rectifying tower (the diameter is less than 1m and the height is more than 60m) and the like are avoided, meanwhile, the tower plate separation efficiency of the rectifying tower is higher, the component separation effect is better, particularly, the purity of the separated diethanol amine is high, the content of the carbon tetrachloride is low, the mixed material preparation is more convenient during the recycling, and each batch of diethanol amine is not required to be detected.
Further optionally, when the amount of the propylene oxide in the reactor is 100kg-200kg, the mass ratio of the amounts of the carbon tetrachloride and the diethanolamine is (0.103-0.129): 1.
further optionally, when the amount of the propylene oxide in the reactor is 1-2 t, the mass ratio of the amounts of the carbon tetrachloride and the diethanolamine is (0.161-0.194): 1.
by adopting the technical scheme, the inventor of the application finds that the input amount of carbon tetrachloride in the process is related to the production scale and the epoxypropane/diethanolamine ratio in the small test and the pilot test, and the more the input amount of carbon tetrachloride is, the better the input amount of carbon tetrachloride is. For example:
for the production period and energy consumption, the increase of the amount of carbon tetrachloride in the reaction material can enhance the effect of promoting the mixing of the propylene oxide and the diethanol amine; however, after the amount of carbon tetrachloride exceeds a threshold value, the improvement of the mixing effect of the epoxypropane and the diethanol amine is promoted to be obviously slowed down or even not promoted continuously, the shortening effect of the mixing time is not promoted, and then the amount of the carbon tetrachloride is increased continuously, so that positive benefits cannot be obtained in terms of heating energy consumption before the mixed material is added into a reactor, refrigeration energy consumption for maintaining the temperature during mixing in the reactor, heating energy consumption during subsequent separation, material cost and conveying power cost, and on the other hand, the reaction rate is reduced due to the dilution effect of the carbon tetrachloride, and the time required by the reaction is prolonged;
for the purity and yield of the product, the consumption of carbon tetrachloride in the reaction materials is increased, the purity and yield of the product can be improved due to the over-intense inhibition effect of the carbon tetrachloride on the local reaction, the consumption is continuously increased, the improvement of the over-intense inhibition effect of the carbon tetrachloride on the local reaction is reflected to the limit of the improvement on the purity of the product, and the reduction of a weaker trend appears after the purity reaches a peak value; the yield is also the same as the reaction result, but the peak value of the yield decrease is not the same as the amount of carbon tetrachloride appearing at the peak value of the purity;
meanwhile, under the production scale magnitude of different quantities, the stirring and mixing prior art influences, different mixed fluid models under different production scales are different, and the better scheme of the production efficiency and the product purity of the diethanol monoisopropanolamine is that proportional joint nodes among carbon tetrachloride, diethanol amine and propylene oxide are different under different production scale magnitudes.
The inventor of the present application determines in the research process that when diethanolamine and propylene oxide are mixed, carbon tetrachloride is mainly affected by the proportion between diethanolamine and propylene oxide and the total amount of diethanolamine and propylene oxide, the product purity and yield are important in the same production period for production, and the inhibition effect of carbon tetrachloride on the side reaction product is considered, the side reaction is mainly caused by polymerization of propylene oxide, propylene oxide tends to react in the production process, so the amount of propylene oxide reflects the amount of heat generated in the reaction process and the amount of side reaction product possibly generated, so the inventor of the present application takes propylene oxide as the second related object of the amount of carbon tetrachloride, tests are performed, and finally the following results are obtained:
when the amount of the propylene oxide in the reactor is 1-2 t, the mass ratio of the amount of the carbon tetrachloride to the amount of the diethanol amine in the reaction materials is (0.161-0.194): 1, the product purity and yield can be better under a short production period;
when the consumption of the epoxy propane in the reactor is 100kg-200kg, the mass ratio of the consumption of the carbon tetrachloride to the consumption of the diethanol amine is (0.103-0.129): 1, the product purity and yield can be better under a short production period;
in the process of gradually enlarging the production scale of the process, the amount ratio of carbon tetrachloride used at the best benefit point of product purity and yield is increased.
Further optionally, graphite powder is mixed in the mixed material, wherein the graphite powder accounts for 0.048-0.062 wt% of the mixed material by mass, and the particle size of the graphite powder is 1-8 μm.
By adopting the technical scheme, when the large-scale production scale is adopted, the graphite powder is mixed in the mixed material, so that the synergistic diethanol amine and the propylene oxide are mixed, the graphite powder moves up and down in liquid in the mixing process, a liquid phase interface is impacted, and the synergistic liquid phase mixing is carried out, so that the purity and the yield of the product are improved in a manner of inhibiting the occurrence of side reactions.
Further optionally, the method further comprises:
s3: after the purification steps including rectification under reduced pressure and solid filtration are carried out on the crude product of the diethanol monoisopropanolamine, obtaining a diethanol monoisopropanolamine product;
the reduced pressure distillation comprises light component separation for separating carbon tetrachloride and other light components and fine separation for separating diethanolamine; and the solid filtering comprises filtering and separating solid matters in a liquid phase after the diethanolamine monoisopropanolamine crude product is finely separated.
In the production process, after graphite powder is mixed in the mixed material, solid precipitate is at the bottom of a liquid phase after the fine separation of the diethanolamine monoisopropanolamine crude product, and the components of the solid precipitate are mainly graphite powder and a high-boiling-point side reaction product.
By adopting the technical scheme, the graphite powder also improves the product purity in a mode of assisting the separation of the high-boiling-point side reaction product from the product. After the light components are separated, the main components of the materials are diethanol monoisopropanolamine and diethanol amine, and trace amount of high-boiling side reaction product impurities. And during fine separation, the diethanolamine is continuously separated, the impurities of the side reaction products with high boiling point are enriched, the graphite powder with the particle size of less than 1 mu m is taken as a nuclear point, and the impurities of the side reaction products with high boiling point are aggregated by taking the graphite powder as the nuclear point, separated from the liquid phase, formed into precipitate and removed by subsequent filtration, so that the graphite powder and the side reaction products with high boiling point are removed from the commodity, and the product purity is improved.
Optionally, the crude diethanolisopropanolamine is filtered to separate graphite powder with a particle size of more than 1 μm from the liquid phase before distillation under reduced pressure.
By adopting the technical scheme, the graphite powder is filtered before reduced pressure distillation, the graphite powder with the particle size larger than 1 mu m is intercepted, and the graphite powder with the particle size smaller than 1 mu m continuously enters the reduced pressure distillation along with the material. Graphite powder with larger grain size (the grain size is not less than 1 mu m) is filtered and separated in advance, so that the problem that the graphite powder is enriched at the bottom of the vacuum distillation tower to influence material circulation and conveying is avoided, and the quality of solid matter filtered after fine separation is reduced.
And further selecting and recycling the graphite powder filtered before the crude diethanol monoisopropanolamine is distilled under reduced pressure.
The desorption of graphite powder to high boiling point side reaction product in this application needs graphite powder to mix together in reaction process along with reaction material, just possesses after making graphite powder surface take place to modify, to the filterable graphite powder before the crude vacuum distillation of diethanol monoisopropanolamine, its surface does not adhere to high boiling point side reaction product and deposits, recycle, reduce cost.
In summary, the present application includes at least one of the following beneficial technical effects:
1. according to the application, diethanolamine and carbon tetrachloride are mixed into a mixed material and melted, and then are uniformly mixed with low-temperature epoxypropane, in the process, carbon tetrachloride promotes diethanolamine to melt, and epoxypropane and diethanolamine to be quickly and efficiently mixed, so that the mixing time is remarkably shortened, the production period is shortened, the energy consumption of refrigeration is reduced, meanwhile, carbon tetrachloride inhibits local reaction from being continuously too intense under the process pressure of the application, the occurrence of local overhigh temperature is reduced, the generation of side reaction is further reduced, and the purity and yield of products are improved;
2. according to the production process, when a large number of production scales are adopted, the graphite powder is mixed into the mixed material, the synergistic material mixing can be performed to inhibit side reactions and assist the separation of high-boiling-point side reaction products, and the purity and the yield of the product are further improved in two aspects.
Detailed Description
Example 1
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: adding propylene oxide with the temperature of 3 ℃ into a reactor, wherein the reactor is a reaction kettle, and the inner volume of the reaction kettle is 1.15m 3 Selecting anchor type stirring slurry with the inner diameter of 1.15m, the diameter D of the slurry of 0.95m and the height h of the slurry of 0.9 m;
the adding amount of the propylene oxide is 116kg, the pressure is regulated by using nitrogen, the pressure in the reaction kettle is regulated to be 0.1MPa, and then the mixed material is added into the reactor;
the temperature of the mixed material is 29 ℃, and the mixed material is pre-mixed diethanolamine and carbon tetrachloride, wherein the dosage of the diethanolamine is 451kg, and the dosage of the carbon tetrachloride is 27.06 kg;
mixing the mixed material with propylene oxide at a stirring speed of 50r/min, keeping the reactor refrigerated, keeping the temperature in the reactor at 5 +/-1 ℃, and mixing for 20min to obtain a reaction material;
s2: heating the reaction materials to 30 ℃, keeping stirring and heating to 70 ℃, maintaining the temperature at 70 +/-1 ℃, and continuing the heat preservation reaction for 2 hours to obtain a crude product of diethanol monoisopropanolamine;
s3: adding the crude product of the diethanol monoisopropanolamine into a distillation still, and separating light components by using a rectifying column separation device, wherein the specification of a rectifying column is as follows: the inner tube h is 50cm, the inner diameter phi is 3cm, the packing is a theta ring, the height of the packing is 32cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature at the bottom of the tower is 70 ℃, and carbon tetrachloride and other light components are separated to obtain a primary separated material;
s4: and (3) adding the primary separated material into another distillation kettle, and performing fine separation by using a rectifying column separation device, wherein the specification of a rectifying column is as follows: the inner tube h is 180cm, the inner diameter phi is 5cm, the packing is a theta ring, the height of the packing is 95cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature of a tower kettle is 156 +/-3 ℃, the temperature at the top of the tower is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine product is obtained after the diethanol amine is separated.
Example 2 to example 7
The production process of diethanol monoisopropanolamine is based on the embodiment 1, the amount of carbon tetrachloride is adjusted, and the process parameters including the specification of a reactor are the same.
Some of the process parameters of examples 1-7 are shown in Table 1 below.
TABLE 1 Process parameter tables of examples 1 to 7
Comparative example 1
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: adding propylene oxide with the temperature of 3 ℃ into a reactor, wherein the reactor is a reaction kettle, and the inner volume of the reaction kettle is 1.15m 3 Selecting anchor type stirring slurry with the inner diameter of 1.15m, the diameter D of the slurry of 0.95m and the height h of the slurry of 0.9 m;
the adding amount of the propylene oxide is 116kg, the pressure is regulated by using nitrogen, the pressure in the reaction kettle is regulated to be 0.1MPa, and then diethanolamine is added into the reactor;
the temperature of the diethanolamine is 29 ℃, and the using amount of the diethanolamine is 451 kg;
mixing diethanolamine and propylene oxide at a stirring speed of 50r/min, keeping the reactor refrigerated, keeping the temperature in the reactor at 5 +/-1 ℃, and mixing for 20min to obtain a reaction material;
s2: heating the reaction materials to 30 ℃, keeping stirring and heating to 70 ℃, maintaining the temperature at 70 +/-1 ℃, and continuing the heat preservation reaction for 2 hours to obtain a crude product of diethanol monoisopropanolamine;
s3: adding the crude product of the diethanol monoisopropanolamine into a distillation still, and separating by using a rectifying column separation device, wherein the specification of a rectifying column is as follows: the inner tube h is 50cm, the inner diameter phi is 3cm, the filler is a theta ring, the height of the filler is 32cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature at the bottom of the tower is 70 ℃, and the light components are separated to obtain a primary separated material;
s4: and (3) adding the primary separated material into another distillation kettle, and separating by using a rectifying column separation device, wherein the specification of the rectifying column is as follows: the inner tube h is 180cm, the inner diameter phi is 5cm, the packing is a theta ring, the height of the packing is 95cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature of a tower kettle is 156 +/-3 ℃, the temperature at the top of the tower is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine product is obtained after the diethanol amine is separated.
Comparative examples 2 to 6
The production process of diethanol monoisopropanolamine is different from comparative example 1 in that the mixing time of diethanol amine and propylene oxide at 5 +/-1 ℃ in comparative examples 2 to 6 is different, and is specifically shown in the following table 2.
Table 2 comparative examples 1 to 6 in which diethanolamine and propylene oxide were mixed at 5. + -. 1 ℃ for a period of time
| Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Mixing time/min | 20 | 30 | 45 | 55 | 65 | 75 |
The intermediate materials of examples 1 to 7 and comparative examples 1 to 3 and diethanolisopropanolamine were tested, and the test contents are as follows.
Reaction material mixing condition detection
Sampling and detecting the prepared reaction materials of each case, wherein sampling sites are random, 20 samples are sampled in each case, and the detection object is determined as the mass percent of diethanol amine due to the fact that liquid volume changes slightly under different temperatures and pressures and propylene oxide is volatile. Taking the mass percent of 20 samples of diethanolamine as a sampling value, taking a theoretical value under the condition that the diethanolamine is completely and uniformly mixed as an average value, calculating relative average deviation, taking the relative average deviation as a reflection index for measuring the mixing condition, wherein the smaller the relative average deviation is, the better the mixing uniformity is, and otherwise, the worse the mixing uniformity is.
Detecting purity and yield
The purity of the obtained diethanolisopropanolamine was checked and the yield was calculated.
The results of the tests on the reaction materials and diethanol monoisopropanolamine in examples 1 to 7 and comparative examples 1 to 6 are shown in Table 3 below.
TABLE 3 Table of the results of the detection of the reactant and diethanolisopropanolamine in examples 1 to 7 and comparative examples 1 to 6
As can be seen from comparative examples 1 to 6, in the prior art, when no carbon tetrachloride is added, the mixing time is increased, the reaction materials are mixed uniformly, the purity and yield of the product are improved along with the increase of the mixing time, and when the mixing time is 65 to 75min, the purity and yield of the product reach better benefits, at the moment, the purity of the product is 95.23 to 95.34 wt%, and the yield of the product is 89.52 to 89.87 wt%.
Comparative examples 1 to 7 and comparative examples 1 to 6.
Compared with the comparative example 1, the product purity and the product yield of the material mixing case of the example 1 are obviously superior to those of the comparative example 1 when the mixing time is the same.
Example 1 compares with comparative example 3, example 1 achieves a similar degree of uniform mixing within a shorter mixing time (20min) as that of comparative example 3 at 45min, while example 1 has a product purity and yield superior to that of comparative example 3.
In comparative examples 1-6, in comparative example 6 with the optimal product purity and yield, the mixing time is 3.75 times that of example 1 in 75min, and the product purity is better than that of example 1 in the application but the product yield is lower than that of example 1; and the product purity of comparative example 6 was still lower than that of example 2.
As can be seen from comparison of examples 1 to 7, in examples 1 to 7, the mixing uniformity is improved continuously as the amount of carbon tetrachloride is increased; the purity and yield of the product are improved with the increase of the amount of carbon tetrachloride before the amount of the carbon tetrachloride reaches 46.63kg, and the purity and yield of the product slowly fall back after the amount of the carbon tetrachloride exceeds 46.63kg, but the purity and yield of the product in example 7 are still better than those in comparative example 6.
Example 4, which is a preferable embodiment, used for mixing for 20min, had a product purity (97.21 wt%), a product yield (93.5 wt%) much higher than that of comparative example 1 (85.2 wt%), and a product yield (75.7 wt%) for the same mixing time, and also superior to that of comparative example 6 (95.34 wt%), and a product yield (89.87 wt%) used for 75min for mixing.
Therefore, in the production process, the carbon tetrachloride and the diethanol amine are mixed into the mixed material in advance, and then the mixed material is mixed with the propylene oxide.
Example 8 example 14
The production process of the diethanol monoisopropanolamine is based on the embodiment 1, the dosage of the epoxypropane, the carbon tetrachloride and the diethanol amine is adjusted, and other process parameters including the specification of a reactor are the same. The amounts of propylene oxide, carbon tetrachloride and diethanolamine are specifically shown in table 4 below.
TABLE 4 parameters of the amounts of propylene oxide, carbon tetrachloride and diethanolamine of example 8 to example 14
| Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | |
| The amount of propylene oxide used per kg | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| Dosage of diethanolamine/kg | 388.79 | 388.79 | 388.79 | 388.79 | 388.79 | 388.79 | 388.79 |
| Amount of carbon tetrachloride/kg | 23.33 | 32.20 | 35.07 | 40.20 | 50.28 | 62.59 | 75.54 |
Comparative example 7
The production process of diethanol monoisopropanolamine is different from that in comparative example 1 in that in comparative example 7, 100kg of epoxy propane is used and 388.79kg of diethanol amine is used.
Example 15 example 21
The production process of diethanol monoisopropanolamine is based on example 1 and is characterized in that a reactor is a reaction kettle, and the internal volume of the reaction kettle is 1.85m 3 The inner diameter is 1.35m, the anchor type stirring slurry is selected, the diameter D of the slurry is 1.2m, the height h of the slurry is 1.1m, the using amounts of the epoxypropane, the carbon tetrachloride and the diethanolamine are adjusted, and other technological parameters are the same.
The amounts of propylene oxide, carbon tetrachloride and diethanolamine are specifically shown in table 5 below.
TABLE 5 parameters of the amounts of propylene oxide, carbon tetrachloride and diethanolamine of example 15 to example 21
| Example 15 | Example 16 | Example 17 | Example 18 | Example 19 | Example 20 | Example 21 | |
| The amount of propylene oxide used per kg | 200 | 200 | 200 | 200 | 200 | 200 | 200 |
| Dosage of diethanolamine/kg | 777.59 | 777.59 | 777.59 | 777.59 | 777.59 | 777.59 | 777.59 |
| Amount of carbon tetrachloride/kg | 46.66 | 64.40 | 70.14 | 80.40 | 100.55 | 125.17 | 151.09 |
Comparative example 8
The difference between the production process of diethanol monoisopropanolamine and the production process of diethanol monoisopropanolamine based on the comparative example 1 is that the internal volume of the reaction kettle in the comparative example 7 is 1.85m 3 The inner diameter is 1.35m, anchor type stirring slurry is selected, the diameter D of the slurry is 1.2m, the height h of the slurry is 1.1m, the dosage of the propylene oxide is 200kg, and the dosage of the diethanolamine is 777.59 kg.
The intermediate materials of examples 8 to 21 and comparative examples 7 to 8 and diethanolisopropanolamine were tested, and the test results are shown in table 6 below.
TABLE 6 Table of the results of the detection of the reaction materials and diethanolisopropanolamine in examples 8 to 21 and comparative examples 7 to 8
| Relative average deviation of reaction material mixing | Purity of the product wt% | Product yield wt% | |
| Example 8 | 0.0860 | 95.69 | 91.77 |
| Example 9 | 0.0257 | 96.84 | 92.96 |
| Example 10 | 0.0199 | 97.47 | 93.38 |
| Example 11 | 0.0153 | 97.44 | 93.71 |
| Example 12 | 0.0131 | 97.26 | 93.52 |
| Example 13 | 0.0113 | 97.15 | 93.49 |
| Example 14 | 0.0110 | 97.06 | 93.33 |
| Comparative example 7 | 0.3090 | 86.70 | 77.20 |
| Example 15 | 0.0990 | 90.59 | 90.52 |
| Example 16 | 0.0359 | 91.62 | 91.76 |
| Example 17 | 0.0258 | 91.91 | 92.17 |
| Example 18 | 0.0203 | 92.12 | 92.24 |
| Example 19 | 0.0165 | 92.11 | 92.35 |
| Example 20 | 0.0152 | 91.92 | 92.27 |
| Example 21 | 0.0141 | 91.75 | 92.11 |
| Comparative example 8 | 0.3740 | 83.50 | 74.30 |
Comparing examples 8-14 and comparative example 7, it is seen that the solution of the present application still achieves good mixing results in shorter mixing times and yields of product better than the prior art given a 100kg dosage schedule of propylene oxide.
Comparing examples 15-21 with comparative example 8, it can be seen that the scheme of the present application can still achieve good mixing effect in a shorter mixing time and yield of product better than the prior art under the planning of 200kg of propylene oxide.
In combination with examples 1-21, it can be seen that the production process of the present application can promote the mixing of propylene oxide and diethanolamine in small-scale experimental production (100kg-200kg of propylene oxide), significantly shorten the mixing time, reduce the refrigeration load, reduce the production cycle, and improve the purity and yield of the product.
According to the examples 1-21, the purity of the product increases and then decreases with the increase of the amount and proportion of carbon tetrachloride, and the yield of the product also increases and then decreases with the increase of the amount and proportion of carbon tetrachloride, but the trends of the two are the same, but the actual maximum peak value is not on the same amount and proportion of carbon tetrachloride.
For examples 1-7, the product yield and purity are optimized near the amount and ratio of carbon tetrachloride in example 4; for examples 8-14, the product purity was optimized near the amount and ratio of carbon tetrachloride for example 10, and the product was optimized near the amount and ratio of carbon tetrachloride for example 12;
for examples 15-21, the product purity was optimized near the amount of carbon tetrachloride, the ratio of example 18, and the product was optimized near the amount of carbon tetrachloride, the ratio of example 19;
therefore, the amount and proportion of carbon tetrachloride can be changed under different amounts, and the material cost is comprehensively considered, so that the amount of carbon tetrachloride and diethanol amine is (0.103-0.129) under the condition that the propylene oxide amount of 100-200kg is used: 1.
example 22
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: will warm upAdding propylene oxide with the temperature of 3 ℃ into a reactor, wherein the reactor is a reaction kettle, and the inner volume of the reaction kettle is 9m 3 Selecting anchor type stirring slurry with the inner diameter of 2.3m, wherein the diameter D of the slurry is 2.1m, and the height h of the slurry is 1.95 m;
the adding amount of the propylene oxide is 1.16t, the pressure is regulated by using nitrogen, the pressure in the reaction kettle is regulated to be 0.12MPa, and then the mixed material is added into the reactor;
the temperature of the mixed material is 29 ℃, and the mixed material is pre-mixed diethanolamine and carbon tetrachloride, wherein the dosage of the diethanolamine is 4.51t, and the dosage of the carbon tetrachloride is 270.6 kg;
mixing the mixed material with propylene oxide at a stirring speed of 50r/min, keeping the reactor refrigerated, keeping the temperature in the reactor at 5 +/-1 ℃, and mixing for 40min to obtain a reaction material;
s2: heating the reaction materials to 30 ℃, keeping stirring and heating to 70 ℃, maintaining the temperature at 70 +/-1 ℃, and continuing the heat preservation reaction for 3 hours to obtain a crude product of diethanol monoisopropanolamine;
s3: adding the crude diethanol monoisopropanolamine into a distillation still, and separating light components by using a rectifying tower separating device, wherein the specification of the rectifying tower is as follows: the inner tube h is 300cm, the inner diameter phi is 35cm, the packing is a theta ring, the height of the packing is 200cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature at the bottom of the tower is 75 ℃, and carbon tetrachloride and other light components are separated to obtain a primary separated material;
s4: and (3) adding the primary separated material into another distillation kettle, and performing rectification separation by using a rectification tower separation device, wherein the specification of the rectification tower is as follows: the inner tube h is 420cm, the inner diameter phi is 50cm, the packing is a theta ring, the height of the packing is 260cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature of a tower kettle is 156 +/-3 ℃, the temperature at the top of the tower is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine product is obtained after the diethanol amine is separated.
Examples 23 to 28
The production process of diethanol monoisopropanolamine is based on the embodiment 1, the amount of carbon tetrachloride is adjusted, and the process parameters including the specification of a reactor are the same.
Some of the process parameters for examples 22-28 are shown in Table 7 below.
TABLE 7 Process parameter tables for examples 22 to 28
Comparative example 9
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: adding propylene oxide with the temperature of 3 ℃ into a reactor, wherein the reactor is a reaction kettle, and the inner volume of the reaction kettle is 9m 3 Selecting anchor type stirring slurry with the inner diameter of 2.3m, wherein the diameter D of the slurry is 2.1m, and the height h of the slurry is 1.95 m;
the adding amount of the propylene oxide is 1.16t, the pressure is regulated by using nitrogen, the pressure in the reaction kettle is regulated to be 0.12MPa, and then diethanolamine is added into the reactor; the temperature of the diethanolamine is 29 ℃, and the using amount is 4.51 t;
mixing diethanolamine and propylene oxide at a stirring speed of 50r/min, keeping the reactor refrigerated, keeping the temperature in the reactor at 5 +/-1 ℃, and mixing for 40min to obtain a reaction material;
s2: heating the reaction materials to 30 ℃, keeping stirring and heating to 70 ℃, maintaining the temperature at 70 +/-1 ℃, and continuing the heat preservation reaction for 3 hours to obtain a crude product of diethanol monoisopropanolamine;
s3: adding the crude diethanol monoisopropanolamine into a distillation still, and separating by using a rectifying tower separation device, wherein the specification of the rectifying tower is as follows: the inner tube h is 300cm, the inner diameter phi is 35cm, the filler is a theta ring, the height of the filler is 200cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature at the bottom of the tower is 75 ℃, and other light components are separated to obtain a primary separated material;
s4: and (3) adding the primary separated material into another distillation kettle, and separating by using a rectifying tower separating device, wherein the specification of the rectifying tower is as follows: the inner tube h is 420cm, the inner diameter phi is 50cm, the packing is a theta ring, the height of the packing is 260cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature of a tower kettle is 156 +/-3 ℃, the temperature at the top of the tower is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine product is obtained after the diethanol amine is separated.
Comparative examples 10 to 14
The production process of diethanol monoisopropanolamine is based on the comparative example 9, and is characterized in that the mixing time of diethanol amine and propylene oxide at 5 +/-1 ℃ is different in the comparative examples 10-14, and the production process is specifically shown in the following table 8.
TABLE 8 comparative examples 9-14 in which diethanolamine and propylene oxide were mixed at 5 + -1 deg.C for a period of time
| Comparative example 9 | Comparative example 10 | Comparative example 11 | Comparative example 12 | Comparative example 13 | Comparative example 14 | |
| Mixing time/min | 40 | 50 | 60 | 70 | 80 | 90 |
The intermediate materials of examples 22 to 28 and comparative examples 9 to 14 and diethanolisopropanolamine were examined.
The results of the examination of the reaction materials and diethanol monoisopropanolamine in examples 22 to 28 and comparative examples 9 to 14 are shown in Table 9 below.
TABLE 9 Table of the results of the examination of the reaction materials and diethanolisopropanolamine in examples 22 to 28 and comparative examples 9 to 14
It can be seen from comparative examples 9-14 that, in the case of no carbon tetrachloride being added in the prior art, when the propylene oxide dosage is on the production scale of 1.16t, the mixing time increases, the better the uniform mixing of the reaction materials is, and the purity and yield of the product increase with the increase of the mixing time.
By comparing examples 22-28 with comparative examples 9-14, the production process of the application mixes the carbon tetrachloride and the diethanolamine into a mixed material in advance and then mixes the mixed material with the propylene oxide, the uniform mixing degree can be achieved when the mixing time in the comparative example is 80min in a short time (40min), and the product purity and the yield are both superior to those in the comparative example.
Therefore, the production process mixes the carbon tetrachloride and the diethanol amine into a mixed material in advance and then mixes the mixed material with the propylene oxide, so that the mixing of the propylene oxide and the diethanol amine can be promoted, the mixing time is obviously shortened, the refrigeration load is reduced, the production period is shortened, and the purity and the yield of the product are improved.
Example 29 example 35
Based on the example 22, the production process of the diethanol monoisopropanolamine adjusts the use amounts of the propylene oxide, the carbon tetrachloride and the diethanol amine, and other process parameters are the same. The amounts of propylene oxide, carbon tetrachloride and diethanolamine are specifically shown in table 10 below.
TABLE 10 parameters for the amounts of propylene oxide, carbon tetrachloride and diethanolamine of examples 29 to 35
| Example 29 | Example 30 | Example 31 | Example 32 | Example 33 | Example 34 | Example 35 | |
| Amount of propylene oxide used/t | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| Dosage of diethanolamine/t | 3.89 | 3.89 | 3.89 | 3.89 | 3.89 | 3.89 | 3.89 |
| Amount of carbon tetrachloride/kg | 233.28 | 321.98 | 350.69 | 401.98 | 502.76 | 625.86 | 755.43 |
Comparative example 15
The production process of diethanol monoisopropanolamine is based on the comparative example 9, and the difference is that the amount of propylene oxide in the comparative example 15 is 1t, and the amount of diethanol amine in the comparative example 15 is 3.89 t.
Example 36 example 42
A process for producing diethanolisopropanolamine, which is based on the embodiment 22 and is characterized in that the inner volume of the reaction kettle is 16m 3 The inner diameter is 2.8m, the anchor type stirring slurry is selected, the diameter D of the slurry is 2.5m, the height h of the slurry is 2.3m, the using amounts of the epoxypropane, the carbon tetrachloride and the diethanolamine are adjusted, and other technological parameters are the same.
The amounts of propylene oxide, carbon tetrachloride and diethanolamine are specifically shown in table 11 below.
TABLE 11 parameters for propylene oxide, carbon tetrachloride and diethanolamine use in examples 36 to 42
| Example 36 | Example 37 | Example 38 | Example 39 | Example 40 | EXAMPLE 41 | Example 42 | |
| Amount of propylene oxide used/t | 2 | 2 | 2 | 2 | 2 | 2 | 2 |
| Dosage of diethanolamine/t | 7.78 | 7.78 | 7.78 | 7.78 | 7.78 | 7.78 | 7.78 |
| Amount of carbon tetrachloride/kg | 466.55 | 643.97 | 701.38 | 803.97 | 1005.52 | 1251.72 | 1510.86 |
Comparative example 16
A process for producing diethanol monoisopropanolamine, which is based on the comparative example 9 and is characterized in that the inner volume of a reaction kettle is 16m 3 The internal diameter is 2.8m, the anchor type stirring slurry is selected, the diameter D of the slurry is 2.5m, the height h of the slurry is 2.3m, the dosage of the propylene oxide is 2t, and the dosage of the diethanolamine is 7.78 t.
The intermediate materials of examples 29 to 42 and comparative examples 15 to 16 and diethanolisopropanolamine were tested, and the results are shown in Table 12 below.
TABLE 12 Table of the results of the examination of the reaction materials and diethanolisopropanolamine in examples 29 to 42 and comparative examples 15 to 16
| Relative average deviation of reaction material mixing | Purity of the product wt% | The product yield is wt% | |
| Example 29 | 0.121 | 89.09 | 90.12 |
| Example 30 | 0.0842 | 94.15 | 91.43 |
| Example 31 | 0.0731 | 95.19 | 91.70 |
| Example 32 | 0.0598 | 96.13 | 91.95 |
| Example 33 | 0.0355 | 97.02 | 92.18 |
| Example 34 | 0.0251 | 97.07 | 92.20 |
| Example 35 | 0.0243 | 97.07 | 92.20 |
| Comparative example 15 | 0.372 | 85.11 | 74.23 |
| Example 36 | 0.157 | 81.73 | 88.23 |
| Example 37 | 0.108 | 91.16 | 90.66 |
| Example 38 | 0.0916 | 93.33 | 91.22 |
| Example 39 | 0.0787 | 94.69 | 91.57 |
| Example 40 | 0.0512 | 96.57 | 92.06 |
| EXAMPLE 41 | 0.0412 | 96.91 | 92.15 |
| Example 42 | 0.0388 | 96.97 | 92.17 |
| Comparative example 16 | 0.3991 | 81.22 | 71.93 |
Comparing examples 28-35 with comparative example 15, it is seen that the solution of the present application still achieves good mixing results in shorter mixing times and yields of product better than the prior art at a dosage of 1t propylene oxide.
Comparing examples 36-42 with comparative example 16, it is seen that the solution of the present application still achieves good mixing results with shorter mixing times and better product purity and yield than the prior art under the 2t propylene oxide dosage schedule.
In combination with examples 22-42, it can be seen that, in the production process of the present application, in a small-scale test (1t-2t of the amount of propylene oxide), the process can promote the mixing of propylene oxide and diethanolamine, reduce the mixing time, reduce the refrigeration load, reduce the side reactions, and improve the purity and yield of the product, and the amount of carbon tetrachloride and diethanolamine is (0.161-0.194): 1.
example 43
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
graphite powder is also added into the mixed material in the S1, the particle size of the graphite powder is 7 +/-1 mu m, and the adding amount of the graphite powder is 3.14 kg;
and (3) filtering the crude diethanolisopropanolamine obtained in the step (S2), and then performing the step (S3), wherein solid matters with the particle size not less than 1 mu m are removed by filtering in the filtering process.
Example 44
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
graphite powder is also added into the mixed material in the S1, the particle size of the graphite powder is 1-2 mu m, and the adding amount of the graphite powder is 3.14 kg;
and (3) filtering the crude diethanolisopropanolamine obtained in the step (S2), and then performing the step (S3), wherein solid matters with the particle size not less than 1 mu m are removed by filtering in the filtering process.
Example 45
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
3.14kg of graphite powder is also added into the mixed material in the S1, wherein the graphite powder is prepared from graphite powder with the particle size of 1-2 mu m and graphite powder with the particle size of 7-8 mu m according to the mass ratio of 1: 1, mixing;
filtering the crude diethanolisopropanolamine obtained from S2, and then performing S3, wherein solid substances with the particle size not less than 1 mu m are removed by filtering in the filtering process;
subsequent production steps are performed.
Example 46
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that: the amount of graphite powder used was 3.88 kg.
Example 47
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that: the amount of graphite powder used was 2.98 kg.
In the processes of examples 43 to 47, it was found that after the fine separation of diethanolamine in the step S4, a little flocculent precipitate appeared in the material, which did not appear in examples 22 to 42, and therefore, it was found that the product was obtained after the filtration of the solid matter from the material after the fine separation of diethanolamine in the step S4 and the removal of the flocculent precipitate by filtration.
The intermediate materials and products obtained in examples 43 to 47 were tested, and the results are shown in Table 13 below.
TABLE 13 Table of the results of detecting the reaction materials and diethanolisopropanolamine in examples 43 to 47
| Relative average deviation of reaction material mixing | Purity of the product wt% | The product yield is wt% | |
| Example 43 | 0.0129 | 98.71 | 94.84 |
| Example 44 | 0.0201 | 99.21 | 94.35 |
| Example 45 | 0.0146 | 99.14 | 94.69 |
| Example 46 | 0.0133 | 99.13 | 94.65 |
| Example 47 | 0.0151 | 99.12 | 94.61 |
In the application, when a large number of production scales are used, graphite powder is mixed into a mixed material, so that synergistic diethanolamine and epoxypropane are mixed, the graphite powder moves up and down in liquid in the mixing process, a liquid phase interface is impacted, synergistic liquid phase mixing is realized, and the product yield is improved.
The addition of graphite powder also plays a further role in promoting the purity of the product.
The precipitate filtered out in examples 43 to 47 was found by composition detection to be a residual graphite powder (particle size less than 1 μm) and a high boiling point side reaction product including an autopolymer of propylene oxide.
The inventor of the application thinks that during fine separation, diethanolamine is continuously separated, the propylene oxide polymer impurities with high boiling point are enriched, and the graphite powder with the particle size smaller than 1 μm is taken as a nucleating agent, so that the propylene oxide polymer impurities with high boiling point are aggregated by taking the graphite powder as a nucleus, separated from a liquid phase and removed in subsequent filtration. Therefore, under the action of graphite powder, the impurities of the propylene oxide polymer with the boiling point higher than that of diethanol amine in the product are removed by combining fine separation and subsequent solid filtration, and the product purity is improved.
For this, the inventor has other schemes in the process of research and development:
comparative example 17
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
silicon dioxide powder is also added into the mixed material in the S1, the particle size of the silicon dioxide powder is 1-2 mu m, and the adding amount of the graphite powder is 3.143 kg;
and (3) filtering the crude diethanolisopropanolamine obtained from the step S2, and then performing the step S3, wherein solid matters with the particle size not less than 1 mu m are removed by filtering in the filtering process.
Comparative example 18
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
silicon dioxide powder is also added into the mixed material in the S1, the particle size of the silicon dioxide powder is 7-8 mu m, and the adding amount of the graphite powder is 3.143 kg;
and (3) filtering the crude diethanolisopropanolamine obtained from the step S2, and then performing the step S3, wherein solid matters with the particle size not less than 1 mu m are removed by filtering in the filtering process.
The intermediate materials and products obtained in comparative examples 17 to 18 were tested, and the test results are shown in Table 14 below.
TABLE 14 detection results of the reaction materials and diethanolisopropanolamine in comparative examples 17 to 18
From the above, it is understood that the use of silica powder is more effective for the mixing of reaction materials, but rather decreases in terms of product purity and product yield, and the inventors analyzed after the study, because the surface of silica activates catalysis for side reactions.
Therefore, the graphite powder is a superior additive for further improving the mixing condition in large-scale production.
To further study the effect of graphite powder, the inventors of the present application also performed the following scheme:
the content of graphite in the solid matter obtained by filtering the material from which the diethanolamine was finely separated in the step S4 in example 45 was detected, and the detection result showed that the content of graphite was 0.0121 kg.
Comparative example 19
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
s4: adding 0.0121kg of graphite powder with the particle size of 0.2 mu m into the primary separation material, uniformly mixing, adding into another distillation kettle, and separating by using a rectifying tower separation device, wherein the specification of the rectifying tower is as follows: the inner tube h is 420cm, the inner diameter phi is 50cm, the packing is theta ring, the height of the packing is 260cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature of a tower kettle is 156 +/-3 ℃, the temperature at the top of the tower is 65-68 ℃, the reflux ratio is 2:1, and after separating the diethanol amine, the materials at the bottom of the tower are filtered to obtain the product of the diethanol monoisopropanolamine.
The purity of the product of comparative example 19 was found to be 97.31 wt%.
Comparative example 20
A process for producing diethanolisopropanolamine, which is based on example 26, and is characterized in that:
s4: adding 0.0121kg of graphite powder with the particle size of 0.05 mu m into the primary separation material, uniformly mixing, adding into another distillation kettle, and separating by using a rectifying tower separation device, wherein the specification of the rectifying tower is as follows: the inner tube h is 420cm, the inner diameter phi is 50cm, the packing is theta ring, the height of the packing is 260cm, the vacuum degree at the top of the tower is 0.09MPa, the temperature of the bottom of the tower is 156 +/-3 ℃, the temperature at the top of the tower is 65-68 ℃, the reflux ratio is 2:1, and after separating the diethanolamine, the materials at the bottom of the tower are filtered to obtain the product of the diethanol monoisopropanolamine.
The purity of the product of comparative example 20 was checked and found to be 97.23 wt%.
The purity of comparative examples 43 to 45 and comparative examples 19 to 20 was not significantly improved. The broken piece of graphite powder source and this preceding reaction in-process graphite powder in the preliminary separation material in the scheme of this application embodiment has produced new surface among the broken piece, and this surface is direct to contact in reaction material, has taken place certain modification in reaction process, so can play the reunion side reaction product, turns into the sediment with it, can be filtered.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: all equivalent changes made according to the structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (8)
1. A production process of diethanol monoisopropanolamine is characterized by comprising the following steps:
s1: adding 2-4 ℃ epoxypropane into a reactor, regulating the pressure with inert gas, wherein the pressure in the reactor is 0.1-0.12 MPa, adding a mixed material into the reactor, wherein the temperature of the mixed material is 28-30 ℃, the total mass ratio of diethanol amine to carbon tetrachloride in the mixed material is more than 99wt%, the mass ratio of diethanol amine to carbon tetrachloride in the mixed material is 1 (0.06-0.2), keeping the reactor refrigerated, keeping the temperature in the reactor at 4-6 ℃, and mixing the epoxypropane and the mixed material until the epoxypropane and the mixed material are uniformly mixed to obtain a reaction material;
s2: and heating the reaction materials to 30 ℃, keeping stirring and heating to 68-72 ℃, maintaining the temperature at 68-72 ℃, and continuing to perform heat preservation reaction for 2-3 hours to obtain a crude product of diethanolisopropanolamine.
2. The process of claim 1, further comprising:
s3: purifying the crude product of the diethanol monoisopropanolamine through a purification step including rectification under reduced pressure to obtain a diethanol monoisopropanolamine product;
the reduced pressure distillation comprises light component separation for separating carbon tetrachloride and other light components and fine separation for separating diethanolamine.
3. The process according to claim 1, wherein the process comprises the following steps: when the dosage of the propylene oxide in the reactor is 100kg-200kg, the dosage mass ratio of the carbon tetrachloride to the diethanolamine is (0.103-0.129): 1.
4. the process according to claim 1, wherein the process comprises the following steps: when the amount of the propylene oxide in the reactor is 1-2 t, the mass ratio of the amount of the carbon tetrachloride to the amount of the diethanol amine is (0.161-0.194): 1.
5. the process according to claim 4, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of:
graphite powder is also mixed in the mixed material, the graphite powder accounts for 0.048-0.062 wt% of the mixed material, and the particle size of the graphite powder is 1-8 mu m.
6. The process of claim 5, further comprising:
s3: after the purification steps including rectification under reduced pressure and solid filtration are carried out on the crude product of the diethanol monoisopropanolamine, obtaining a diethanol monoisopropanolamine product;
the reduced pressure distillation comprises light component separation for separating carbon tetrachloride and other light components and fine separation for separating diethanolamine;
and the solid filtering comprises filtering and separating solid matters in a liquid phase after the diethanolamine monoisopropanolamine crude product is finely separated.
7. The process according to claim 6, wherein the production process of diethanol monoisopropanolamine comprises the following steps: filtering to separate graphite powder with the particle size of more than 1 mu m from a liquid phase before carrying out reduced pressure distillation on the crude diethanolisopropanolamine.
8. The process according to claim 7, wherein the reaction is carried out in the presence of a catalyst selected from the group consisting of: and (3) recycling the graphite powder filtered before the crude diethanol monoisopropanolamine is subjected to reduced pressure distillation.
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