CN114835593B - Production process of diethanol monoisopropanolamine - Google Patents
Production process of diethanol monoisopropanolamine Download PDFInfo
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- CN114835593B CN114835593B CN202210483438.4A CN202210483438A CN114835593B CN 114835593 B CN114835593 B CN 114835593B CN 202210483438 A CN202210483438 A CN 202210483438A CN 114835593 B CN114835593 B CN 114835593B
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- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
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- C—CHEMISTRY; METALLURGY
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- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
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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 propylene oxide with the temperature of 2-4 ℃ into a reactor, wherein the pressure in the reactor is 0.1-0.12 MPa, adding a mixed material with the temperature of 28-30 ℃, wherein the total mass ratio of diethanolamine to carbon tetrachloride in the mixed material is more than 99wt%, 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 propylene oxide and the mixed material until the reaction material is uniformly obtained; the reaction materials are heated to 30 ℃, the stirring and the heating are kept to 68-72 ℃, the temperature is kept to keep the heat preservation reaction 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, is widely used in cement additives and carbon dioxide capturing agents, has high requirements on the purity of the diethanol monoisopropanolamine in the use process, and is researched from the aspects of process routes, material mixing, separation and purification of products and the like in the production process of the diethanol monoisopropanolamine in industry.
At present, the popular research direction is to produce the product by taking diethanolamine and propylene oxide as raw materials. And taking the reaction kettle as a reactor, adding diethanolamine into propylene oxide with the temperature lower than 10 ℃, mixing the two, and inhibiting side reaction at a low temperature to generate side reaction products with high boiling point. After diethanolamine is dissolved or uniformly dispersed in propylene oxide, the temperature is raised to react, so that the reaction positions in the reactor are almost uniformly distributed in the mixed materials, the reaction contact is more sufficient, the main reaction rate is high, the occurrence of side reaction propylene oxide is less, and finally the product diethanol monopropanolamine is obtained after reduced pressure distillation.
The inventors have found in experiments directed to the related art as described above:
the melting point of the diethanolamine at normal pressure is 28 ℃, the diethanolamine is mixed with the propylene oxide at the temperature below 10 ℃, and then the diethanolamine is quickly cooled and solidified after contacting the propylene oxide, so that the mixing speed between the diethanolamine and the propylene oxide is slow, and meanwhile, the temperature in the reactor is controlled by external cooling in the mixing process, so that the mixing speed is further restricted, and even if the mechanical stirring is provided by the prior industrial technology, the mixing of the diethanolamine and the propylene oxide is completed for a long time, so that the problem of long actual production period is caused.
Disclosure of Invention
The application provides a production process of diethanol monoisopropanolamine in order to improve the production efficiency of diethanol monoisopropanolamine synthesized by diethanol and epoxypropane.
The production process of the diethanol monoisopropanolamine provided by the application adopts the following technical scheme:
a production process of diethanol monoisopropanolamine comprises the following steps:
s1: adding propylene oxide with the temperature of 2-4 ℃ into a reactor, regulating the pressure of the inert gas, keeping the pressure in the reactor at 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 diethanolamine and carbon tetrachloride in the mixed material is more than 99wt%, the mass ratio of diethanolamine and 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 propylene oxide and the mixed material until the mixed material is uniformly mixed to obtain a reaction material;
s2: heating the reaction material to 30 ℃, keeping stirring and heating to 68-72 ℃, keeping the temperature at 68-72 ℃, and continuing to perform heat preservation reaction for 2-3 h to obtain the crude product of the diethanol monoisopropanolamine.
By adopting the technical scheme:
the diethanolamine and the carbon tetrachloride are firstly mixed into a mixed material, and the carbon tetrachloride dissolves the diethanolamine and accelerates the diethanolamine to be melted in the process of heating the mixed material to 28-30 ℃; after being mixed into a liquid mixed material, the carbon tetrachloride reduces the solidifying point of the mixed material and slows down the solidification phenomenon caused by the contact of the mixed material with low-temperature propylene oxide;
when the mixed material is mixed with propylene oxide, the carbon tetrachloride can promote the mutual dissolution of the propylene oxide and the diethanol amine, and even when the temperature of the reactor is maintained at 4-6 ℃, the carbon tetrachloride can promote the rapid and efficient mixing of the propylene oxide and the diethanol amine, thereby obviously shortening the mixing time, shortening the production period and reducing the refrigeration energy consumption.
On the other hand, after the mixture is uniformly mixed with propylene oxide to obtain a reaction material, the temperature of the reaction material is raised, the main reaction of synthesizing diethanol monoisopropanolamine by propylene oxide and diethanol amine rapidly occurs, the reaction is exothermic, and the temperature of the reaction material continuously rises along with the reaction. In the actual production process, although a cooling device is used for controlling the temperature in the reactor, the controlled reaction temperature is determined by a feedback mechanism and is actually the whole temperature in the reactor or the reflection result of the temperature of a plurality of sites in the reactor, the situation that the local temperature is too high due to the fact that the main reaction is too hard at the local sites still exists in the reactor, and the side reaction is also aggravated at the local sites due to the fact that the local temperature is too high. The occurrence of the local overhigh temperature is difficult to prevent, namely, the local reaction is too violent, the concentration is reduced along with the reaction due to the concentration enrichment of a certain area, the reaction is slowed down, the temperature is reduced, the prior art can not realize the mixed preparation of single molecules and single molecule-to-molecule levels, and the local reaction is too violent and inevitably occurs but is unexpected.
The carbon tetrachloride added in the application is close to the optimal temperature for reaction control and is higher than the optimal temperature for reaction control and lower than the boiling point of diethanolamine and diethanol monoisopropanolamine under the process pressure of the application, so that the local temperature is too high due to the overviolent local reaction, the heat energy in the carbon tetrachloride rapid absorption area in the area is used as the latent heat, the liquid state is converted into the gas state with the same temperature, the reaction heat generated by diethanol monoisopropanolamine is transferred, the local reaction is restrained from continuing to be overviolent, the occurrence of the local temperature is reduced, the occurrence of side reaction is further reduced, and the purity and the yield of the product are improved.
Further optionally, the method further comprises:
s3: the crude product of the diethanol monoisopropanolamine is subjected to a purification step including reduced pressure rectification to obtain a diethanol monoisopropanolamine product; the reduced pressure distillation comprises light component separation for separating carbon tetrachloride and other light components, and refined separation for separating diethanolamine.
By adopting the technical scheme, the separation of carbon tetrachloride and other light components and the separation of diethanolamine are divided into two steps by the reduced pressure distillation and purification of the crude product of the diethanol monoisopropanolamine, the equipment requirement is reduced, the simultaneous separation of the light components, carbon tetrachloride, diethanolamine and diethanol monoisopropanolamine in a single rectifying tower/rectifying column is avoided, the unsuitable and unreasonable equipment design requirements of a giant rectifying tower (with the diameter of more than 5 m) or a fine high rectifying tower (with the diameter of less than 1m and the height of more than 60 m) and the like are avoided, the tray separation efficiency of the rectifying tower is higher, the component separation effect is better, the purity of the separated diethanolamine is high, the carbon tetrachloride content is less, the preparation of mixed materials during recycling is more convenient, and the detection of each batch of diethanolamine is not needed.
Further alternatively, when the dosage of the cyclopropane in the reactor is 100kg-200kg, the dosage mass ratio of the carbon tetrachloride to the diethanolamine is (0.103-0.129): 1.
further alternatively, when the dosage of the cyclopropane in the reactor is 1-2 t, the dosage mass ratio of the carbon tetrachloride to the diethanolamine is (0.161-0.194): 1.
by adopting the technical scheme, the inventor discovers that the input amount of carbon tetrachloride in the process is related to the production scale and the ratio of propylene oxide to diethanolamine in the small test and pilot test processes, and the larger the input amount of carbon tetrachloride is, the better the input amount of carbon tetrachloride is. For example:
for the production period and the energy consumption, the increase of the carbon tetrachloride consumption in the reaction materials can enhance the effect of promoting the mixing of propylene oxide and diethanolamine; however, after the amount of carbon tetrachloride exceeds a threshold, the improvement of the mixing effect of propylene oxide and diethanolamine is obviously slowed down and even is not continuously improved, the shortening effect of the mixing time is not improved, and after that, the continuous increase of the amount of carbon tetrachloride can not obtain forward benefits for the energy consumption of heating before adding the mixed materials into the reactor, the refrigeration energy consumption of maintaining the temperature during mixing in the reactor, the heating energy consumption during subsequent separation, the material cost and the conveying power cost, and on the other hand, the reaction rate is reduced due to the dilution effect of the carbon tetrachloride, and the reaction time is prolonged;
regarding the purity and yield of the product, the dosage of carbon tetrachloride in the reaction materials is increased, the purity and yield of the product are improved due to the excessively strong inhibition effect of carbon tetrachloride on the local reaction, then the dosage is continuously increased, the excessively strong inhibition effect of carbon tetrachloride on the local reaction is improved and reflected on the improvement trend limit of the purity of the product, the reduction of weaker trend appears after the purity reaches the peak value, and the inventor considers that the increase is probably due to the excessive dosage of carbon tetrachloride, the influence on the reduction of the progress of the main reaction caused by the dilution of the raw materials of the diethanol monopropanol amine synthesized by propylene oxide and diethanol amine is larger than the influence on the uniformly mixed progress of the main reaction; the yield is the same reaction result, but the peak value of the yield inverse reduction is not the same as the carbon tetrachloride amount of the purity peak value;
meanwhile, under the production scale of different volume, the method is influenced by the stirring and mixing prior art, the mixed fluid model under different production scales is different, and the ratio joint nodes among carbon tetrachloride, diethanolamine and propylene oxide are different under different production scale of better schemes of the production efficiency and the product purity of the diethanol monoisopropanolamine.
The inventor confirms in the research process that when diethanolamine is mixed with propylene oxide, carbon tetrachloride is mainly influenced by the proportion between diethanolamine and propylene oxide and the total consumption of diethanolamine and propylene oxide, the purity and the yield of the product are important in the same production period, and the side reaction mainly causes the propylene oxide to react in the production process due to the polymerization of propylene oxide under the consideration of the inhibition influence of carbon tetrachloride on the side reaction products, so the amount of propylene oxide reflects the heating amount in the reaction process and the possible amount of the side reaction products, and the inventor takes propylene oxide as a second related object of the carbon tetrachloride consumption to carry out experiments to finally obtain the product:
when the dosage of the cyclopropane in the reactor is 1-2 t, the dosage mass ratio of the carbon tetrachloride to the diethanolamine in the reaction materials is (0.161-0.194): 1, obtaining better product purity and yield under a short production period;
when the dosage of the cyclopropane in the reactor is 100kg-200kg, the dosage mass ratio of the carbon tetrachloride to the diethanol amine is (0.103-0.129): 1, obtaining better product purity and yield under a short production period;
in the gradual expansion process of the production scale of the process, the carbon tetrachloride dosage ratio used at the best point of the benefit of the product purity and the yield is increased.
Further alternatively, graphite powder is mixed in the mixed material, wherein the graphite powder accounts for 0.048-0.062 wt% of the mass of the mixed material, and the particle size of the graphite powder is 1-8 mu m.
By adopting the technical scheme, when the production scale is large, the mixing of the graphite powder in the mixed material is beneficial to the mixing of the synergistic diethanolamine and the propylene oxide, namely the graphite powder moves up and down in the liquid in the mixing process, impacts the liquid phase interface and the synergistic liquid phase is mixed, so that the purity and the yield of the product are improved in a mode of inhibiting side reaction.
Further optionally, the method further comprises:
s3: the crude product of the diethanol monoisopropanolamine is subjected to a purification step including vacuum rectification and solid filtering to obtain a diethanol monoisopropanolamine product;
the reduced pressure distillation comprises light component separation for separating carbon tetrachloride and other light components, and refined separation for separating diethanolamine; the solid filtering comprises filtering and separating solid matters in a liquid phase after the refined separation of the crude product of the diethanolamine monoisopropanolamine.
In the production process, after graphite powder is mixed in the mixed material, solid precipitation exists at the bottom of a liquid phase after refined separation of the crude product of the diethanolamine monoisopropanolamine, and the solid precipitation component mainly comprises the graphite powder and high-boiling-point side reaction products.
By adopting the technical scheme, the graphite powder also improves the purity of the product in a mode of assisting the separation of the high-boiling-point side reaction product from the product. The main components of the materials after the separation of the light components are diethanol monoisopropanolamine and diethanol amine, and trace impurities of side reaction products with high boiling points are also contained. During fine separation, diethanolamine is continuously separated, high-boiling point side reaction product impurities are enriched, graphite powder with the particle size smaller than 1 mu m is taken as a nuclear point, the high-boiling point side reaction product impurities are aggregated by taking the graphite powder as a nuclear, are separated from a liquid phase to form precipitates, and are removed by subsequent filtration, so that the graphite powder and the high-boiling point side reaction products are removed from the commodity, and the product purity is improved.
Further alternatively, the crude product of diethanol monoisopropanolamine is filtered to separate graphite powder with the particle size of more than 1 mu m from a liquid phase before reduced pressure distillation.
By adopting the technical scheme, the graphite powder is filtered before reduced pressure distillation, the graphite powder with the grain diameter larger than 1 mu m is trapped, and the graphite powder with the grain diameter smaller than 1 mu m continuously enters the reduced pressure distillation along with the material. Graphite powder with larger particle size (particle size is not less than 1 mu m) is filtered and separated in advance, so that the influence of enrichment of the graphite powder at the bottom of a vacuum distillation tower on material circulation and transportation is avoided, and on the other hand, the quality of filtered solid matters after fine separation is reduced.
Further alternatively, the graphite powder filtered before the distillation of the crude product of the diethanol monoisopropanolamine is recycled.
The removal of the high-boiling point side reaction products by the graphite powder is realized by mixing the graphite powder together with the reaction materials in the reaction process, so that the surface of the graphite powder is modified, the graphite powder filtered before the distillation of the crude product of the diethanol monoisopropanolamine under reduced pressure is not attached with the precipitation of the high-boiling point side reaction products, and the graphite powder can be recycled and the cost is reduced.
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 firstly mixed into a mixed material and melted, and then the mixed material is uniformly mixed with low-temperature propylene oxide, so that during the process, the carbon tetrachloride promotes the diethanolamine to be melted, and the rapid and efficient mixing of the propylene oxide and the diethanolamine is promoted, so that the mixing time is obviously shortened, the production period is shortened, the refrigeration energy consumption is reduced, and meanwhile, the carbon tetrachloride is under the process pressure, the partial reaction is restrained from continuing to be too violent, the occurrence of the partial temperature is reduced, the occurrence of side reaction is further reduced, and the purity and the yield of the product are improved;
2. when the production process is used in large-scale production, graphite powder is mixed in the mixed materials, so that the mixed materials can be used for enhancing the mixing of the materials to inhibit side reactions and assist the separation of high-boiling-point side reaction products, and the purity and the yield of the products are further improved.
Detailed Description
Example 1
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: propylene oxide with the temperature of 3 ℃ is added into a reactor, the reactor is a reaction kettle, and the internal volume of the reaction kettle is 1.15m 3 Inner diameter of1.15m, selecting an anchor stirring paddle, wherein the diameter D of the paddle is 0.95m, and the height h of the paddle is 0.9m;
the addition amount of 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 ℃, 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 27.06kg;
mixing the mixed material with propylene oxide, stirring at a speed of 50r/min, cooling the reactor, maintaining the temperature in the reactor at 5+/-1 ℃, and mixing for 20min to obtain a reaction material;
s2: heating the reaction material to 30 ℃, keeping stirring and heating to 70 ℃, keeping the temperature at 70+/-1 ℃, and continuing to perform heat preservation reaction for 2 hours to obtain a crude product of the diethanol monoisopropanolamine;
s3: adding the diethanol monoisopropanolamine crude product into a distillation kettle, and separating light components by utilizing a rectifying column separating device, wherein the rectifying column has the specification: the inner pipe h=50cm, the inner diameter phi=3cm, the packing is theta-ring, the packing height is 32cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 70 ℃, and the primary separation material is obtained after separating carbon tetrachloride and other light components;
s4: adding the primary separation material into another distillation kettle, and performing rectification separation by utilizing a rectification column separation device, wherein the rectification column has the specification: the inner pipe h=180 cm, the inner diameter phi=5 cm, the packing is theta rings, the packing height is 95cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 156+/-3 ℃, the tower top temperature is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine is separated to obtain the product diethanol monoisopropanolamine.
Example 2-example 7
The production process of the diethanol monoisopropanolamine is based on the embodiment 1, the dosage of carbon tetrachloride is adjusted, and the technological parameters including the specification of the reactor are the same.
Some of the process parameters for examples 1-7 are shown in Table 1 below.
TABLE 1 Process parameter tables for examples 1-7
Comparative example 1
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: propylene oxide with the temperature of 3 ℃ is added into a reactor, the reactor is a reaction kettle, and the internal volume of the reaction kettle is 1.15m 3 The inner diameter is 1.15m, an anchor stirring paddle is selected, the diameter D of the paddle is 0.95m, and the height h of the paddle is 0.9m;
the addition amount of 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 dosage is 451kg;
mixing diethanolamine and propylene oxide, stirring at a speed of 50r/min, cooling the reactor, maintaining the temperature in the reactor at 5+/-1 ℃, and mixing for 20min to obtain a reaction material;
s2: heating the reaction material to 30 ℃, keeping stirring and heating to 70 ℃, keeping the temperature at 70+/-1 ℃, and continuing to perform heat preservation reaction for 2 hours to obtain a crude product of the diethanol monoisopropanolamine;
s3: adding the crude product of the diethanol monoisopropanolamine into a distillation kettle, and separating by utilizing a rectifying column separating device, wherein the specification of the rectifying column is as follows: the inner pipe h=50cm, the inner diameter phi=3cm, the packing is theta-ring, the packing height is 32cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 70 ℃, and the primary separation material is obtained after the light components are separated;
s4: adding the primary separation material into another distillation kettle, and separating by using a rectifying column separating device, wherein the specification of the rectifying column is as follows: the inner pipe h=180 cm, the inner diameter phi=5 cm, the packing is theta rings, the packing height is 95cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 156+/-3 ℃, the tower top temperature is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine is separated to obtain the product diethanol monoisopropanolamine.
Comparative examples 2 to 6
The production process of diethanol monoisopropanolamine is different from that of comparative example 1 in that the mixing time of diethanol amine and propylene oxide in comparative examples 2 to 6 is different at 5+ -1deg.C, and is specifically shown in the following Table 2.
TABLE 2 mixing time of diethanolamine with propylene oxide at 5.+ -. 1 ℃ in comparative examples 1 to 6
| 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 and diethanol monoisopropanolamine of examples 1 to 7 and comparative examples 1 to 3 were tested as follows.
Detection of mixing condition of reaction materials
The prepared reaction materials of each case are sampled and detected, sampling sites are random, and 20 samples are sampled for each case, and the detection object is determined as the mass percent of diethanolamine because of the trace change of the liquid volume and the volatile volatilization of propylene oxide under different temperatures and pressures. The mass percent of diethanolamine of 20 samples is taken as a sampling value, the theoretical value under the condition that the diethanolamine is completely and uniformly mixed is taken as an average value, the relative average deviation is calculated, the relative average deviation is taken as a reflecting index for measuring the mixing condition, the smaller the relative average deviation is, the better the mixing uniformity degree is, and otherwise, the worse the mixing uniformity degree is.
Purity and yield detection
The purity of the obtained diethanol monoisopropanolamine is detected and the yield is calculated.
The results of the detection of the reaction materials and the diethanol monoisopropanolamine of 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 reaction materials and the diethanol monoisopropanolamine of examples 1 to 7 and comparative examples 1 to 6
As is clear from comparative examples 1 to 6, in the case of no carbon tetrachloride addition in the prior art, the better the mixing uniformity of the reaction materials is, the higher the purity and yield of the product are, the better the benefit is achieved when the mixing time is 65 to 75min, the purity of the product is 95.23 to 95.34wt% and the yield of the product is 89.52 to 89.87wt%.
Comparative examples 1 to 7 and comparative examples 1 to 6.
In the case of the mixture of the materials in example 1, the product purity and the product yield are obviously better than those in comparative example 1 in comparison with comparative example 1 at the same mixing time.
Example 1 compared to comparative example 3, example 1 achieved a similar degree of uniformity of mixing in a shorter mixing time (20 min) than 45min in comparative example 3, whereas example 1 had better product purity and yield than significant comparative example 3.
Comparative examples 6, in which the purity and yield of the product were optimal, were 3.75 times as high as those of example 1 in 75 minutes for mixing, and the purity of the product was higher than that of example 1 of the present application but the yield of the product was lower than that of example 1; and the purity of the product of comparative example 6 was still lower than that of example 2.
As can be seen from comparative examples 1 to 7, examples 1 to 7 were improved continuously with increasing amounts of carbon tetrachloride; the purity and yield of the product increased with increasing carbon tetrachloride amount until the carbon tetrachloride amount reached 46.63kg, and slowly fallen back after the carbon tetrachloride amount exceeded 46.63kg, but the purity and yield of the product of example 7 remained better than that of comparative example 6.
As a preferable embodiment, example 4 was 20min at the time of mixing, and its product purity (97.21 wt%), product yield (93.5 wt%) were far higher than that of comparative example 1 at the same mixing time (85.2 wt%), product yield (75.7 wt%), and also better than that of comparative example 6 at 75min at the time of mixing (95.34 wt%), product yield (89.87 wt%).
Therefore, in the production process, the carbon tetrachloride and the diethanolamine are mixed into the mixed material in advance, and then the mixed material is mixed with the epoxypropane, so that the process can promote the mixing of the epoxypropane and the diethanolamine, obviously shorten the mixing time, reduce the refrigeration load, reduce the production period, and simultaneously improve the purity and the yield of the product.
Example 8-example 14
The production process of the diethanol monoisopropanolamine is based on the embodiment 1, the dosages of propylene oxide, carbon tetrachloride and diethanol amine are adjusted, and other process parameters including the specification of the reactor are the same. The amounts of propylene oxide, carbon tetrachloride and diethanolamine are shown in Table 4.
TABLE 4 propylene oxide, carbon tetrachloride, diethanolamine consumption parameters for examples 8-14
| Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | |
| Propylene oxide dosage/kg | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| Diethanolamine dosage/kg | 388.79 | 388.79 | 388.79 | 388.79 | 388.79 | 388.79 | 388.79 |
| Carbon tetrachloride amount/kg | 23.33 | 32.20 | 35.07 | 40.20 | 50.28 | 62.59 | 75.54 |
Comparative example 7
A process for producing diethanol monoisopropanolamine differs from comparative example 1 in that the amount of propylene oxide used in comparative example 7 is 100kg and the amount of diethanol amine used is 388.79kg.
Example 15-example 21
A production process of diethanol monoisopropanolamine is based on the embodiment 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, an anchor stirring slurry is selected, the slurry diameter D is 1.2m, the slurry height h is 1.1m, and the dosages of propylene oxide, carbon tetrachloride and diethanolamine are regulated, and other technological parameters are the same.
The amounts of propylene oxide, carbon tetrachloride and diethanolamine are shown in Table 5.
TABLE 5 propylene oxide, carbon tetrachloride, diethanolamine consumption parameters for examples 15-21
| Example 15 | Example 16 | Example 17 | Example 18 | Example 19 | Example 20 | Example 21 | |
| Propylene oxide dosage/kg | 200 | 200 | 200 | 200 | 200 | 200 | 200 |
| Diethanolamine dosage/kg | 777.59 | 777.59 | 777.59 | 777.59 | 777.59 | 777.59 | 777.59 |
| Carbon tetrachloride amount/kg | 46.66 | 64.40 | 70.14 | 80.40 | 100.55 | 125.17 | 151.09 |
Comparative example 8
The production process of the diethanol monoisopropanolamine is based on the comparative example 1, and is different in that the internal volume of a reaction kettle in the comparative example 7 is 1.85m 3 The inner diameter is 1.35m, an anchor stirring slurry is selected, the slurry diameter D is 1.2m, the slurry height h is 1.1m, the dosage of propylene oxide is 200kg, and the dosage of diethanolamine is 777.59kg.
The intermediate materials and diethanol monoisopropanolamine of examples 8 to 21 and comparative examples 7 to 8 were examined, and the examination results are shown in Table 6 below.
TABLE 6 Table of the results of the detection of the reaction materials and the diethanol monoisopropanolamine of examples 8 to 21 and comparative examples 7 to 8
| Relative average deviation of the mixing conditions of the reaction materials | The purity of the product is wt% | The yield of the product is 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 |
Comparative examples 8-14 and comparative example 7 show that the inventive procedure still achieves good mixing results in a shorter mixing time and yields better than the prior art with a 100kg propylene oxide dosage schedule.
Comparative examples 15-21 and comparative example 8 show that the inventive protocol still achieves good mixing results in a shorter mixing time and yields better than the prior art with a 200kg propylene oxide dosage schedule.
As can be seen from examples 1-21, the production process of the application can promote mixing of propylene oxide and diethanolamine in small-scale test production (100 kg-200kg propylene oxide consumption), remarkably shorten mixing time, reduce refrigeration load, reduce production period, and improve purity and yield of the product.
According to examples 1-21, the product purity increased with increasing carbon tetrachloride amount and duty ratio and then decreased, and the product yield increased with increasing carbon tetrachloride amount and duty ratio and then decreased, but the trend of the two was the same, but the actual maximum peak was not on the same carbon tetrachloride amount and duty ratio.
For examples 1-7, the product yield, purity was optimized around the carbon tetrachloride amount, duty cycle of example 4; for examples 8-14, the purity of the product was optimized near the carbon tetrachloride amount and the duty cycle of example 10, and the product was optimized near the carbon tetrachloride amount and the duty cycle of example 12;
for examples 15-21, the purity of the product was optimized near the carbon tetrachloride amount and the duty cycle of example 18, and the product was optimized near the carbon tetrachloride amount and the duty cycle of example 19;
therefore, the dosage and the ratio of the carbon tetrachloride can be changed under different dosages, and the material cost is comprehensively considered, and the dosage of the carbon tetrachloride and the diethanol amine is (0.103-0.129) under the dosage scale of 100-200kg of the epoxypropane: 1.
example 22
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: propylene oxide with the temperature of 3 ℃ is added into a reactor, the reactor is a reaction kettle, and the internal volume of the reaction kettle is 9m 3 Inner, innerThe diameter is 2.3m, an anchor stirring paddle is selected, the diameter D of the paddle is 2.1m, and the height h of the paddle is 1.95m;
the addition amount of 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 ℃, 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 270.6kg;
mixing the mixed material with propylene oxide, stirring at a speed of 50r/min, cooling the reactor, maintaining the temperature in the reactor at 5+/-1 ℃, and mixing for 40min to obtain a reaction material;
s2: heating the reaction material to 30 ℃, keeping stirring and heating to 70 ℃, keeping the temperature at 70+/-1 ℃, and continuing to perform heat preservation reaction for 3 hours to obtain a crude product of the diethanol monoisopropanolamine;
s3: adding the crude product of the diethanol monoisopropanolamine into a distillation kettle, and separating light components by utilizing a rectifying tower separating device, wherein the specification of the rectifying tower is as follows: the inner pipe h=300 cm, the inner diameter phi=35 cm, the packing is theta-rings, the packing height is 200cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 75 ℃, and the primary separation material is obtained after separating carbon tetrachloride and other light components;
s4: adding the primary separation material into another distillation kettle, and performing rectification separation by utilizing a rectifying tower separation device, wherein the specification of the rectifying tower is as follows: the inner pipe h=420 cm, the inner diameter phi=50cm, the packing is theta rings, the packing height is 260cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 156+/-3 ℃, the tower top temperature is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine is separated to obtain the product diethanol monoisopropanolamine.
Examples 23 to 28
The production process of the diethanol monoisopropanolamine is based on the embodiment 1, the dosage of carbon tetrachloride is adjusted, and the technological parameters including the specification of the 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 22-28
Comparative example 9
A production process of diethanol monoisopropanolamine comprises the following steps:
s1: propylene oxide with the temperature of 3 ℃ is added into a reactor, the reactor is a reaction kettle, and the internal volume of the reaction kettle is 9m 3 The inner diameter is 2.3m, an anchor stirring paddle is selected, the diameter D of the paddle is 2.1m, and the height h of the paddle is 1.95m;
the addition amount of 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 dosage is 4.51t;
mixing diethanolamine and propylene oxide, stirring at a speed of 50r/min, cooling the reactor, maintaining the temperature in the reactor at 5+/-1 ℃, and mixing for 40min to obtain a reaction material;
s2: heating the reaction material to 30 ℃, keeping stirring and heating to 70 ℃, keeping the temperature at 70+/-1 ℃, and continuing to perform heat preservation reaction for 3 hours to obtain a crude product of the diethanol monoisopropanolamine;
s3: adding the crude product of the diethanol monoisopropanolamine into a distillation kettle, separating by utilizing a rectifying tower separating device, and obtaining the specification of the rectifying tower: the inner pipe h=300 cm, the inner diameter phi=35 cm, the packing is theta-rings, the packing height is 200cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 75 ℃, and the primary separation material is obtained after other light components are separated;
s4: adding the primary separation 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 pipe h=420 cm, the inner diameter phi=50cm, the packing is theta rings, the packing height is 260cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 156+/-3 ℃, the tower top temperature is 65-68 ℃, the reflux ratio is 2:1, and the diethanol amine is separated to obtain the product diethanol monoisopropanolamine.
Comparative examples 10 to 14
A production process of diethanol monoisopropanolamine is based on comparative example 9, and is different in that the mixing time of diethanol amine and propylene oxide in comparative examples 10-14 is different at 5+/-1 ℃, and the specific mixing time is shown in the following table 8.
TABLE 8 mixing time of diethanolamine with propylene oxide at 5.+ -. 1 ℃ in comparative examples 9-14
| 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 were examined for diethanol monoisopropanolamine.
The results of the detection of the reaction materials and the diethanol monoisopropanolamine of examples 22 to 28 and comparative examples 9 to 14 are shown in Table 9 below.
TABLE 9 Table of the results of the detection of the reaction materials and the diethanol monoisopropanolamine in examples 22 to 28 and comparative examples 9 to 14
As is clear from comparative examples 9 to 14, in the case of no carbon tetrachloride addition in the prior art, the better the mixing uniformity of the reaction materials, the higher the purity and yield of the product as the mixing time increases, when the propylene oxide amount is increased at a production scale of 1.16 t.
By comparing examples 22 to 28 with comparative examples 9 to 14, the production process of the application mixes carbon tetrachloride and diethanolamine into a mixture in advance and then mixes the mixture with propylene oxide, and can achieve similar mixing uniformity when the mixing time is 80min in the comparative example in a shorter time (40 min), and meanwhile, the purity and the yield of the product are both superior to those of the comparative example.
Therefore, the production process of the application mixes the carbon tetrachloride and the diethanol amine into the mixture in advance and then mixes the mixture with the epoxypropane, thereby promoting the mixing of the epoxypropane and the diethanol amine, obviously shortening the mixing time, reducing the refrigeration load, reducing the production period and simultaneously improving the purity and the yield of the product.
Examples 29 to 35
The production process of the diethanol monoisopropanolamine is based on the embodiment 22, the dosages of propylene oxide, carbon tetrachloride and diethanol amine are adjusted, and other process parameters are the same. The amounts of propylene oxide, carbon tetrachloride and diethanolamine are shown in Table 10.
TABLE 10 propylene oxide, carbon tetrachloride, diethanolamine consumption parameters for examples 29-35
| Example 29 | Example 30 | Example 31 | Example 32 | Example 33 | Example 34 | Example 35 | |
| Propylene oxide dosage/t | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| Amount of diethanolamine/t | 3.89 | 3.89 | 3.89 | 3.89 | 3.89 | 3.89 | 3.89 |
| Carbon tetrachloride amount/kg | 233.28 | 321.98 | 350.69 | 401.98 | 502.76 | 625.86 | 755.43 |
Comparative example 15
A production process of diethanol monoisopropanolamine is based on comparative example 9, and the difference is that the amount of the epoxy propane in comparative example 15 is 1t, and the amount of the diethanol amine is 3.89t.
Examples 36 to 42
The production process of diethanol monoisopropanolamine is based on example 22, and is different in that the internal volume of the reaction kettle is 16m 3 The inner diameter is 2.8m, an anchor stirring slurry is selected, the slurry diameter D is 2.5m, the slurry height h is 2.3m, and the dosages of propylene oxide, carbon tetrachloride and diethanolamine are regulated, and other technological parameters are the same.
The amounts of propylene oxide, carbon tetrachloride and diethanolamine are shown in Table 11.
TABLE 11 propylene oxide, carbon tetrachloride, diethanolamine consumption parameters for examples 36-42
| Example 36 | Example 37 | Example 38 | Example 39 | Example 40 | Example 41 | Example 42 | |
| Propylene oxide dosage/t | 2 | 2 | 2 | 2 | 2 | 2 | 2 |
| Amount of diethanolamine/t | 7.78 | 7.78 | 7.78 | 7.78 | 7.78 | 7.78 | 7.78 |
| Carbon tetrachloride amount/kg | 466.55 | 643.97 | 701.38 | 803.97 | 1005.52 | 1251.72 | 1510.86 |
Comparative example 16
The production process of the diethanol monoisopropanolamine is based on comparative example 9, and is different in that the internal volume of the reaction kettle is 16m 3 The inner diameter is 2.8m, an anchor stirring slurry is selected, the slurry diameter D is 2.5m, the slurry height h is 2.3m, the dosage of propylene oxide is 2t, and the dosage of diethanolamine is 7.78t.
The intermediate materials of examples 29 to 42 and comparative examples 15 to 16 and diethanol monoisopropanolamine were examined, and the examination results are shown in Table 12 below.
TABLE 12 Table of the results of the detection of the reaction materials and the diethanol monoisopropanolamine in examples 29 to 42 and comparative examples 15 to 16
| Relative average deviation of the mixing conditions of the reaction materials | The purity of the product is wt% | The yield of the product 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 |
Comparative examples 28-35 and comparative example 15 show that the inventive protocol still achieves good mixing results in a shorter mixing time and yields better than the prior art with a 1t propylene oxide dosage schedule.
Comparative examples 36-42 and comparative example 16 show that the inventive protocol still achieves good mixing results in a shorter mixing time and yields better than the prior art with a 2t propylene oxide dosage schedule.
As can be seen from the combination of examples 22-42, the production process of the application can promote the mixing of propylene oxide and diethanolamine in small-scale test production (the dosage of 1t-2t propylene oxide), reduce the mixing time, reduce the refrigeration load, simultaneously reduce side reactions, improve the purity and the yield of the product, and the dosage of carbon tetrachloride and diethanolamine is (0.161-0.194): 1.
example 43
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that:
the mixed material in the step S1 is also added with graphite powder, the particle size of the graphite powder is 7+/-1 mu m, and the adding amount of the graphite powder is 3.14kg;
and (3) filtering the crude product of the diethanol monoisopropanolamine obtained in the step (S2) and then carrying out the step (S3), and filtering in the filtering process to remove solid matters with the particle size not smaller than 1 mu m.
Example 44
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that:
the mixed material in the step S1 is also added with graphite powder, the particle size of the graphite powder is 1-2 mu m, and the adding amount of the graphite powder is 3.14kg;
and (3) filtering the crude product of the diethanol monoisopropanolamine obtained in the step (S2) and then carrying out the step (S3), and filtering in the filtering process to remove solid matters with the particle size not smaller than 1 mu m.
Example 45
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that:
3.14kg of graphite powder is also added into the mixture in the step S1, and 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 product of the diethanol monoisopropanolamine obtained in the step S2, and then carrying out the step S3, wherein solid matters with the particle size not smaller than 1 mu m are removed through filtration in the filtering process;
subsequent production steps are carried out.
Example 46
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that: the graphite powder was used in an amount of 3.88kg.
Example 47
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that: the graphite powder was used in an amount of 2.98kg.
In the process of examples 43 to 47, it was found that a small amount of solid flocculent precipitate was present in the material after the diethanolamine was finely separated in the step S4, which was not present in examples 22 to 42, and therefore the material after the diethanolamine was finely separated in the step S4 was filtered for solid matter, and the product was obtained after the solid flocculent precipitate was removed by filtration.
The intermediate materials and products obtained in examples 43 to 47 were examined, and the examination results are shown in Table 13 below.
TABLE 13 Table of results of detection of reaction materials and diethanol monoisopropanolamine for examples 43 to 47
| Relative average deviation of the mixing conditions of the reaction materials | The purity of the product is wt% | The yield of the product 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, graphite powder is mixed into the mixed material in order to increase the efficiency of the mixture of diethanolamine and propylene oxide when the large-scale production scale is realized, the graphite powder moves up and down in the liquid in the mixing process, impacts the liquid phase interface, increases the efficiency of the liquid phase mixture, and improves the product yield.
The addition of graphite powder also has a further promoting effect on the purity of the product.
The precipitate filtered out in examples 43-47 was found to be a residual graphite powder (particle size less than 1 μm) and a high boiling side reaction product, including a self-polymer of propylene oxide, by component detection.
The inventors believe that during the fine separation, diethanolamine is continuously separated, the high boiling propylene oxide polymer impurities are enriched, the graphite powder with the particle size smaller than 1 μm is used as a nuclear agent at this time, the high boiling propylene oxide polymer impurities are gathered by using the graphite powder as a nucleus, are separated from the liquid phase, and are removed in the subsequent filtration. Therefore, under the action of graphite powder, the propylene oxide polymer impurities with boiling points higher than that of diethanolamine in the product are removed by combining fine separation and subsequent solid filtering, so that the purity of the product is improved.
Other schemes exist in the research and development process of the inventor:
comparative example 17
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that:
silicon dioxide powder with the particle size of 1-2 mu m and the addition of 3.143kg is added into the mixture in the step S1;
and (3) filtering the crude product of the diethanol monoisopropanolamine obtained in the step (S2) and then carrying out the step (S3), and filtering in the filtering process to remove solid matters with the particle size not smaller than 1 mu m.
Comparative example 18
A process for the production of diethanol monoisopropanolamine, based on example 26, differs in that:
silicon dioxide powder with the particle size of 7-8 mu m and the addition of 3.143kg is added into the mixture in the step S1;
and (3) filtering the crude product of the diethanol monoisopropanolamine obtained in the step (S2) and then carrying out the step (S3), and filtering in the filtering process to remove solid matters with the particle size not smaller than 1 mu m.
The intermediate materials and products obtained in comparative examples 17 to 18 were examined, and the examination results are shown in Table 14 below.
TABLE 14 Table of results for the detection of comparative examples 17 to 18 reaction mass and diethanol monoisopropanolamine
From the above, it is clear that the use of silica powder is better for the mixing of the reaction materials, but it is rather reduced in terms of product purity and product yield, which the inventors have studied for post-analysis-due to the surface of silica activating the catalysis of side reactions.
Therefore, the graphite powder is an additive superior product for further improving the mixing condition under the mass production.
To further investigate the effect of graphite powder, the present inventors have also carried out the following scheme:
the graphite content in the solid matter obtained by filtering the material after the refined separation of diethanolamine in the step S4 in the example 45 was detected, and the graphite content was 0.0121kg.
Comparative example 19
A process for the production of diethanol monoisopropanolamine, based on example 26, differs 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 still, and separating by using a rectifying tower separating device, wherein the specification of the rectifying tower is as follows: the inner pipe h=420 cm, the inner diameter phi=50cm, the packing is theta rings, the packing height is 260cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 156+/-3 ℃, the tower top temperature is 65-68 ℃, the reflux ratio is 2:1, and the product diethanol monoisopropanolamine is obtained by filtering the tower bottom material after the diethanol amine is separated.
The purity of the product of comparative example 19 was examined and found to be 97.31% by weight.
Comparative example 20
A process for the production of diethanol monoisopropanolamine, based on example 26, differs 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, separating by using a rectifying tower separating device, and obtaining the specification of the rectifying tower: the inner pipe h=420 cm, the inner diameter phi=50cm, the packing is theta rings, the packing height is 260cm, the tower top vacuum degree is 0.09MPa, the tower bottom temperature is 156+/-3 ℃, the tower top temperature is 65-68 ℃, the reflux ratio is 2:1, and the product diethanol monoisopropanolamine is obtained by filtering the tower bottom material after the diethanol amine is separated.
The purity of the product of comparative example 20 was examined and found to be 97.23% by weight.
The purity of comparative examples 43 to 45 and comparative examples 19 to 20 was not significantly improved. According to the scheme provided by the embodiment of the application, graphite powder sources in the materials are initially separated from fragments generated by crushing graphite powder in the previous reaction process, a new surface is generated in the fragment crushing process, the surface is directly contacted with the reaction materials, and certain modification is carried out in the reaction process, so that the agglomeration side reaction products can be obtained, converted into precipitates and filtered.
The above embodiments are not intended to limit the scope of the present application, so: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (4)
1. The production process of the diethanol monoisopropanolamine is characterized by comprising the following steps of:
s1: adding propylene oxide with the temperature of 2-4 ℃ into a reactor, regulating the pressure of 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 diethanolamine and carbon tetrachloride in the mixed material is more than 99wt%, the mass ratio of diethanolamine and carbon tetrachloride in the mixed material is 1 (0.06-0.2), keeping the reactor refrigerated, maintaining the temperature in the reactor at 4-6 ℃, and mixing the propylene oxide and the mixed material until the mixed material is uniformly mixed to obtain a reaction material;
s2: heating the reaction material 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 the diethanol monoisopropanolamine;
the dosage of the cyclopropane in the reactor is 1-2 t, and the dosage mass ratio of the carbon tetrachloride to the diethanol amine is (0.161-0.194): 1, the mixed material is also mixed with graphite powder, the graphite powder accounts for 0.048-0.062wt% of the mass of the mixed material, and the particle size of the graphite powder is 1-8 mu m.
2. The production process of diethanol monoisopropanolamine according to claim 1, further comprising:
s3: the crude product of the diethanol monoisopropanolamine is subjected to a purification step including vacuum rectification and solid filtering to obtain a diethanol monoisopropanolamine product;
the vacuum rectification sequentially comprises light component separation for separating carbon tetrachloride and other light components and fine separation for separating diethanolamine;
the solid filtering comprises filtering and separating solid matters in a liquid phase after the refined separation of the crude product of the diethanolamine monoisopropanolamine.
3. The production process of diethanol monoisopropanolamine according to claim 2, characterized in that: before the crude product of diethanol monoisopropanolamine is decompressed and rectified, graphite powder with the particle size larger than 1 mu m is separated from a liquid phase by filtering.
4. A process for the production of diethanol monoisopropanolamine according to claim 3, characterized in that: and recycling the graphite powder filtered before the decompression rectification of the crude product of the diethanol monoisopropanolamine.
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