CN105601539A - Reaction and purification system and process for aliphatic or alicyclic dicarbamate - Google Patents
Reaction and purification system and process for aliphatic or alicyclic dicarbamate Download PDFInfo
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- CN105601539A CN105601539A CN201610212173.9A CN201610212173A CN105601539A CN 105601539 A CN105601539 A CN 105601539A CN 201610212173 A CN201610212173 A CN 201610212173A CN 105601539 A CN105601539 A CN 105601539A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C269/00—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C269/04—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups from amines with formation of carbamate groups
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Abstract
The invention discloses a reaction and purification system and process for aliphatic or alicyclic dicarbamate, comprising a gas-liquid mixed reaction kettle, a thin-film evaporator and a tail gas absorber, wherein the gas-liquid mixed reaction kettle comprises a kettle body provided with a waste gas outlet, a gas inlet and a reaction product outlet, the thin-film evaporator is communicated with the reaction product outlet, the tail gas absorber is communicated with the waste gas outlet; the gas-liquid mixed reaction kettle also comprises a stirrer and a plurality of first gas distributors, the stirrer comprises a plurality of stirring paddles and a stirring shaft; the first gas distributors are arranged below the stirring paddles; the lower end of the stirring shaft is a hollow part of which a first end is communicated with a gas inlet pipe by the gas inlet of the kettle body, and a second end of the hollow part is positioned between the stirring paddles and the first gas distributors. The reaction and purification system provided by the invention has the advantages of high reaction conversion efficiency, small dissipation of energy, high purity of product purified, convenience of recovery and treatment of byproduct gas, lower cost and simple operation, and is suitable for industrialized big production of carbamate compounds.
Description
Technical field
The invention belongs to chemical field, relate to a kind of chemical intermediate preparation technology, specifically, relate to reaction and purification system and the technique of a kind of aliphatic or ring family diurethane.
Background technology
Isocyanates is the important organic compound of a class, is the primary raw material of synthesis of polyurethane. Fat (ring) family diurethane is as its reaction intermediate. Carrying out synthesis of carbamates by alcoholysis of urea is the approach that has prospects for commercial application at present most. But existing method, as DE3200559 needs high temperature, high pressure, reaction time long, reaction selectivity is poor, and product yield is low; US3013064 adopts Cu(OAc) as catalyst synthesis of carbamates, reaction pressure is high, and productive rate is lower than 80%; CN01106723.3 adopts nano-metal-oxide synthesis of carbamates, but the carbamate that its important intermediate N for synthesizing isocyanate replaces is inapplicable; In patent CN1231463C, utilize PbO, KOH, ZnCl2、Pd/C、HZSM5、HY、CH3The catalysis aniline such as OK, urea and alcohol reaction synthesizing phenyl carbamate, although mild condition, catalyst amount is very large, and activity is not high, conversion ratio only has 20% left and right, does not possess industrialized condition.
Therefore, need that research and development are a kind of comes the new technology of synthesis of carbamates and reaction, purification system by alcoholysis of urea badly, it is easy and simple to handle, and accessory substance is few, and conversion ratio is high, selectively good, and does not need to add expensive catalyst.
Summary of the invention
Technical problem to be solved by this invention is to provide reaction and purification system and the technique of the carbamate that a kind of reaction conversion ratio is high, energy consumption is little, raw material by-product recovery is processed conveniently, cost is lower, easy and simple to handle.
For achieving the above object, the invention provides a kind of reaction and purification system of producing aliphatic or ring family diurethane, this reaction and purification system comprise:
Gas-liquid mixed reactor, it comprises kettle, and the top of this kettle is provided with outlet port, and the bottom of this kettle is respectively arranged with air inlet and reacting product outlet;
With the luwa evaporator that the reacting product outlet of gas-liquid mixed reactor is communicated with by pump, this luwa evaporator has charging aperture, top light component discharging opening, bottom heavy constituent discharging opening;
The tail gas absorber being communicated with the outlet port of gas-liquid mixed reactor;
Described gas-liquid mixed reactor also comprises:
Be arranged on the agitator in kettle, this agitator comprises some paddles and a shaft;
Be arranged on some the first gas distributors under described paddle;
Wherein, described shaft has hollow part, it is arranged on the lower end of shaft, the first end of this hollow part is communicated with admission line by the air inlet of kettle, the second end of this hollow part is between described paddle and the first gas distributor, and the first described gas distributor is communicated with admission line by the hollow part of shaft.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, this gas-liquid mixed reactor also comprises:
Be arranged on kettle outside, be connected to the first condensing unit on the outlet port of kettle, this first condensing unit has: the exhaust outlet being communicated with tail gas absorber, the steam inlet being connected with the outlet port of gas-liquid mixed reactor, the condensate liquid refluxing opening being communicated with kettle.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, the afterbody of this first condensing unit is also provided with stop valve.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, the outside of described kettle is also provided with heater.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, described paddle is six leaf disc turbine-like.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, described paddle is staggered to be connected with the first gas distributor and is arranged on shaft.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, the first described gas distributor is the circular tube shaped thing of one end sealing, the tube wall of this first gas distributor arranges some apertures; Preferably, on every the first gas distributor the summation of foraminate sectional area be more than or equal to the sectional area of this first gas distributor pipe caliber.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, the outside of described luwa evaporator is also provided with the second condensing unit being connected with the top discharge mouth of described luwa evaporator.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, described luwa evaporator also comprises:
Be communicated with the light component gathering-device of the outlet of the second condensing unit;
Be communicated with the heavy constituent receiving system of the bottom heavy constituent discharging opening of luwa evaporator.
Reaction and the purification system of above-mentioned aliphatic or ring family diurethane, wherein, described tail gas absorber comprises:
Tower body, the middle part of this tower body is filled with filler, and the bottom of this tower body fills exhaust-gas treatment solution;
Be arranged on the second gas distributor of tower body bottom, this second gas distributor is communicated with the outlet port of gas-liquid mixed reactor;
Be arranged on the spray equipment at tower body top, by circulating pump, the exhaust-gas treatment solution of locating of bottom, absorption tower be pumped into spray equipment.
The present invention also provides a kind of technique of preparing aliphatic or ring family diurethane, and this technique comprises following steps:
Step 1, by aliphatic/ring family diamines, urea, fatty alcohol and ionic liquid are with molar ratio computing 1:(1 ~ 5): (1 ~ 10): (1 ~ 6) is placed in gas-liquid mixed reactor, pass into nitrogen replacement air, reaction temperature is 150 DEG C ~ 350 DEG C, reaction pressure 0.5MPa ~ 3MPa, air inlet by reactor bottom passes into nitrogen, make the gas-liquid of raw material in kettle evenly mix and get rid of the accessory substance ammonia generating through the first gas distributor, reclaim through tail gas absorber, reaction time is 1 ~ 15h, one pot reaction is prepared aliphatic/ring family diurethane, wherein, described aliphatic/ring family diamines selects 1, 4-cyclohexane diamine, hexamethylene diamine, 4, 4'-diamino-dicyclohexyl methane, IPD, trimethyl hexamethylene diamine, any one in norbornane dimethylamine, described fatty alcohol is saturation unit fatty alcohol, described ionic liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl diethyldithiocarbamate ether-3-methyl imidazolium tetrafluoroborate, 1-ethyl acetate base-3-methylimidazole hexafluorophosphate, 1-butyl-2,3-methylimidazole bromine salt, tributyl octyl group bromide phosphine, 1-are fluoro-2, one or more combinations in 6-dichloropyridine tetrafluoroborate, 1-butyl-3-picoline tetrafluoroborate, 4-ethyl-4-methyl morpholine bromine salt, 1-ethyl-3-methylimidazole bis trifluoromethyl sulfimide salt,
Step 2, is transferred to the product of step 1 in luwa evaporator by pump, separating-purifying light component and heavy constituent, and this light component refers to fatty alcohol solvent; This heavy constituent refers to aliphatic or ring family's diurethane and ionic liquid.
Reaction provided by the invention and purification system reaction conversion ratio is high, energy consumption is little, raw material by-product recovery is processed convenient (separating and then reclaim respectively fatty alcohol and ionic liquid by luwa evaporator, absorption tower recycling accessory substance ammonia); Technological operation provided by the invention is easy, does not need to add catalyst, can significantly reduce fatty alcohol solvent, and cost is lower, is applicable to the industrialized production of carbamate.
Brief description of the drawings
Fig. 1 is a kind of aliphatic or the reaction of ring family diurethane and structural representation of purification system produced provided by the invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, by specific embodiment, the invention will be further described, and these embodiment, for the present invention is described, are not only limiting the scope of the invention.
This reaction and purification system comprise: through reactor, luwa evaporator and tail gas absorber particular design, that have good gas-liquid mixed effect. Wherein, reactor has gas phase mouth, liquid return hole, heat exchanger and bottom discharge mouth; Material after reaction finishes is squeezed into luwa evaporator through measuring pump and is removed the remaining light component of minute quantity (butanols etc.), and the jar that heavy constituent (aliphatic or ring family's diurethane and ionic liquid) flows into below stores for future use; The ammonia that reaction produces passes into tail gas absorber bottom, and inner dilute sulfuric acid is got to spray head above by pump, and middle part part has filler, can make dilute sulfuric acid liquid fully contact absorption with unabsorbed ammonia.
As shown in Figure 1, be a kind of reaction and purification system of preparing aliphatic diamino acid ester type compound provided by the invention, this reaction and purification system comprise:
The invention provides a kind of reaction and purification system of producing aliphatic or ring family diurethane, this reaction and purification system comprise:
Gas-liquid mixed reactor 10, it comprises kettle 11, and the top of this kettle 11 is provided with outlet port 111, and the bottom of this kettle is respectively arranged with air inlet 112 and reacting product outlet 113, and this air inlet 112 is changed by threeway with reacting product outlet 113;
With the luwa evaporator 20 that the reacting product outlet 113 of gas-liquid mixed reactor is communicated with by pump 30, this luwa evaporator 20 has charging aperture 21, top light component discharging opening 22, bottom heavy constituent discharging opening 23;
The tail gas absorber 40 being communicated with the outlet port 111 of gas-liquid mixed reactor;
Described gas-liquid mixed reactor 10 also comprises:
Be arranged on the agitator 12 in kettle, this agitator comprises some paddles 121 and a shaft 122;
Be arranged on some the first gas distributors 13 under described paddle 121;
Wherein, described shaft 122 has hollow part, it is arranged on the lower end of shaft 122, the first end of this hollow part is communicated with admission line by the air inlet 112 of kettle, the second end of this hollow part is between described paddle 121 and the first gas distributor 13, and the first described gas distributor 13 is communicated with admission line by the hollow part of shaft.
In some embodiment, described gas-liquid mixed reactor 10 also comprises:
Be arranged on kettle outside, be connected to the first condensing unit 14(on the outlet port 111 of kettle horizontal or vertical), this first condensing unit 14 has: the exhaust outlet 141 being communicated with tail gas absorber, the steam inlet 142 being connected with the outlet port of gas-liquid mixed reactor, the condensate liquid refluxing opening 143 being communicated with kettle.
In some embodiment, the afterbody of the first described condensing unit 14 is also provided with stop valve 144.
In some embodiment, the outside of described kettle is also provided with heater 15.
In some embodiment, described paddle 121 is six leaf disc turbine-like.
In some embodiment, described paddle 121 is staggered to be connected with the first gas distributor 13 and is arranged on shaft 122.
In some embodiment, the first described gas distributor 13 is the circular tube shaped thing of one end sealing, and the tube wall of this first gas distributor arranges some apertures; Preferably, on every the first gas distributor the summation of foraminate sectional area be more than or equal to the sectional area of this first gas distributor pipe caliber.
In some embodiment, the outside of described luwa evaporator 20 is also provided with the second condensing unit 24 being connected with the top discharge mouth 22 of described luwa evaporator.
In some embodiment, described luwa evaporator 20 also comprises:
Be communicated with the light component gathering-device 25 of the outlet of the second condensing unit;
Be communicated with the heavy constituent receiving system 26 of the bottom heavy constituent discharging opening of luwa evaporator.
In some embodiment, described tail gas absorber 40 comprises:
Tower body 41, the middle part of this tower body 41 is filled with filler, the optional stainless steel of this filler, the random packing of the materials such as pottery, PE or PP, form of bio-carrier is Pall ring, Raschig ring, rectangular saddle ring or cascade ring etc.; The bottom of this tower body 41 fills exhaust-gas treatment solution;
The second gas distributor 42 that is arranged on tower body bottom, this second gas distributor 42 is communicated with the outlet port 111 of gas-liquid mixed reactor;
Be arranged on the spray equipment 43 at tower body top, by circulating pump, the exhaust-gas treatment solution of locating of bottom, absorption tower be pumped into spray equipment 43.
The reaction process that adopts reaction of the present invention and purification system to prepare aliphatic diamino acid ester type compound illustrates by following examples.
Embodiment 1:
By 100kg IPD, 78kg urea, it is in the new-type gas-liquid mixed reactor of 500L that 96kg n-butanol and 100kg1-ethyl-3-methylimidazole tetrafluoroborate add volume, logical N2Air in displacement still. Under mechanical agitation, be warming up to 280 DEG C, start to get rid of from the logical nitrogen of autoclave body bottom the ammonia that reaction generates, this gas removes tail gas absorber through still heat exchange of top part device, during this, keep pressure is wherein 0.5-2.5MPa always, is incubated sampling after 8 hours, carries out HPLC analysis, IPD conversion ratio approximately 100%, major product isophorone diamino acid butyl ester is selective 95%, stops reaction, closes nitrogen and stirring. Open afterwards the rotor of luwa evaporator, the circulatory mediator chilled water of vavuum pump unit and heat exchanger, evaporimeter internal pressure maintains-70 ~-100KPa. The now valve of crack autoclave body bottom, making material enter luwa evaporator purifies, 8.2kg butanols gas enters the condensation of evaporimeter heat exchange of top part device and reclaims, and it is for subsequent use that 206kg isophorone diamino acid butyl ester and 100kg ionic liquid 1-ethyl-3-methylimidazole tetrafluoroborate fall into the storage tank of base of evaporator.
Embodiment 2:
By 100kg IPD, 78kg urea, 60kg ethanol and 100kg1-butyl-2, it is in the new-type gas-liquid mixed reactor of 500L that 3-methylimidazole bromine salt adds volume, air in logical N2 displacement still. Under mechanical agitation, be warming up to 280 DEG C, start to get rid of from the logical nitrogen of autoclave body bottom the ammonia that reaction generates, this gas removes tail gas absorber through still heat exchange of top part device, during this, keep pressure is wherein 1.5-3.0MPa always, is incubated sampling after 8 hours, carries out HPLC analysis, IPD conversion ratio approximately 100%, major product isophorone diamino acid butyl ester is selective 98%, stops reaction, closes nitrogen and stirring. Open afterwards the rotor of luwa evaporator, the circulatory mediator chilled water of vavuum pump unit and heat exchanger, evaporimeter internal pressure maintains-70 ~-100KPa. The now valve of crack autoclave body bottom, making material enter luwa evaporator purifies, 5.8kg alcohol gas enters the condensation of evaporimeter heat exchange of top part device and reclaims, 185kg isophorone diamino acid ethyl ester and 100kg ionic liquid 1-butyl-2, it is for subsequent use that 3-methylimidazole bromine salt falls into the storage tank of base of evaporator.
Embodiment 3:
By 80kg diamines, 92kg urea, it is in the new-type gas-liquid mixed reactor of 500L that 113kg n-butanol and 80kg1-ethyl-3-methylimidazole tetrafluoroborate add volume, air in logical N2 displacement still. Under mechanical agitation, be warming up to 250 DEG C, start to get rid of from the logical nitrogen of autoclave body bottom the ammonia that reaction generates, this gas removes tail gas absorber through still heat exchange of top part device, and during this, keep pressure is wherein 1.0-2.0MPa always, is incubated sampling after 6 hours, carry out HPLC analysis, diamines conversion ratio approximately 100%, major product 1,6-hexa-methylene diamino butyl formate selective 96%, stop reaction, close nitrogen and stirring. Open afterwards the rotor of luwa evaporator, the circulatory mediator chilled water of vavuum pump unit and heat exchanger, evaporimeter internal pressure maintains-70 ~-100KPa. The now valve of crack autoclave body bottom, making material enter luwa evaporator purifies, 10.8kg butanols gas enters the condensation of evaporimeter heat exchange of top part device and reclaims, 209kg1, it is for subsequent use that 6-hexa-methylene diamino butyl formate and 80kg ionic liquid 1-ethyl-3-methylimidazole tetrafluoroborate fall into the storage tank of base of evaporator.
Embodiment 4:
By 80kg diamines, 92kg urea, it is in the new-type gas-liquid mixed reactor of 500L that 49kg methyl alcohol and 80kg4-ethyl-4-methyl morpholine bromine salt add volume, air in logical N2 displacement still. Under mechanical agitation, be warming up to 250 DEG C, start to get rid of from the logical nitrogen of autoclave body bottom the ammonia that reaction generates, this gas removes tail gas absorber through still heat exchange of top part device, and during this, keep pressure is wherein 1.0-2.0MPa always, is incubated sampling after 6 hours, carry out HPLC analysis, diamines conversion ratio approximately 100%, major product 1,6-hexa-methylene diamino-methyl formate selective 99%, stop reaction, close nitrogen and stirring. Open afterwards the rotor of luwa evaporator, the circulatory mediator chilled water of vavuum pump unit and heat exchanger, evaporimeter internal pressure maintains-70 ~-100KPa. The now valve of crack autoclave body bottom, making material enter luwa evaporator purifies, 4.8kg methanol gas enters the condensation of evaporimeter heat exchange of top part device and reclaims, 158kg1, it is for subsequent use that 6-hexa-methylene diamino-methyl formate and 80kg ionic liquid 4-ethyl-4-methyl morpholine bromine salt fall into the storage tank of base of evaporator.
Embodiment 5:
By 80kg1,4-cyclohexanediamine, 93kg urea, it is in the new-type gas-liquid mixed reactor of 500L that 114kg n-butanol and 80kg1-ethyl-3-methylimidazole bis trifluoromethyl sulfimide salt add volume, air in logical N2 displacement still. Under mechanical agitation, be warming up to 220 DEG C, start to get rid of from the logical nitrogen of autoclave body bottom the ammonia that reaction generates, this gas removes tail gas absorber through still heat exchange of top part device, and during this, keep pressure is wherein 2.0-3.0MPa always, be incubated sampling after 4 hours, carry out HPLC analysis, Isosorbide-5-Nitrae-cyclohexanediamine conversion ratio approximately 100%, major product 1,4-hexamethylene diamino acid butyl ester is selective 92%, stops reaction, closes nitrogen and stirring. Open afterwards the rotor of luwa evaporator, the circulatory mediator chilled water of vavuum pump unit and heat exchanger, evaporimeter internal pressure maintains-70 ~-100KPa. The now valve of crack autoclave body bottom, making material enter luwa evaporator purifies, 10.0kg methanol gas enters the condensation of evaporimeter heat exchange of top part device and reclaims, 202kg1, it is for subsequent use that 4-hexamethylene diamino acid butyl ester and 80kg ionic liquid 1-ethyl-3-methylimidazole bis trifluoromethyl sulfimide salt fall into the storage tank of base of evaporator.
Embodiment 6:
By 120kg4,4'-diamino-dicyclohexyl methane, 76kg urea, it is in the new-type gas-liquid mixed reactor of 500L that 76kg normal propyl alcohol and 120kg1-ethyl acetate base-3-methylimidazole hexafluorophosphate add volume, air in logical N2 displacement still. Under mechanical agitation, be warming up to 180 DEG C, start to get rid of from the logical nitrogen of autoclave body bottom the ammonia that reaction generates, this gas removes tail gas absorber through still heat exchange of top part device, and during this, keep pressure is wherein 0.6-1.8MPa always, be incubated sampling after 10 hours, carry out HPLC analysis, 4,4'-diamino-dicyclohexyl methane conversion ratio approximately 100%, major product 4,4'-dicyclohexyl methyl hydride diamino acid propyl ester is selective 89%, stops reaction, closes nitrogen and stirring. Open afterwards the rotor of luwa evaporator, the circulatory mediator chilled water of vavuum pump unit and heat exchanger, evaporimeter internal pressure maintains-70 ~-100KPa. The now valve of crack autoclave body bottom, making material enter luwa evaporator purifies, 7.4kg normal propyl alcohol gas enters the condensation of evaporimeter heat exchange of top part device and reclaims, 194kg4, it is for subsequent use that 4'-dicyclohexyl methyl hydride diamino acid propyl ester and 80kg ionic liquid 1-ethyl acetate base-3-methylimidazole hexafluorophosphate fall into the storage tank of base of evaporator.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention. Read after foregoing those skilled in the art, for multiple amendment of the present invention and substitute will be all apparent. Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. reaction and the purification system of aliphatic or ring family diurethane, is characterized in that, this reaction and purification system comprise:
Gas-liquid mixed reactor (10), it comprises kettle (11), and the top of this kettle (11) is provided with outlet port (111), and the bottom of this kettle (11) is respectively arranged with the air inlet (112) and reacting product outlet (113) through threeway conversion;
With the luwa evaporator (20) that the reacting product outlet of gas-liquid mixed reactor (10) is communicated with by pump (30), this luwa evaporator (20) has charging aperture (21), top light component discharging opening (22), bottom heavy constituent discharging opening (23);
The tail gas absorber (40) being communicated with the outlet port (111) of gas-liquid mixed reactor (10);
Described gas-liquid mixed reactor (10) also comprises:
Be arranged on the agitator (12) in kettle (11), this agitator (12) comprises some paddles (121) and a shaft (122);
Be arranged on (122) on shaft, be positioned at some the first gas distributors (13) under described paddle (121);
Wherein, described shaft (122) has hollow part, it is arranged on the lower end of shaft (122), the first end of this hollow part is communicated with admission line by the air inlet (112) of kettle, the second end of this hollow part is positioned between described paddle (121) and the first gas distributor (13), and described the first gas distributor (13) is communicated with admission line by the hollow part of shaft.
2. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, is characterized in that, this gas-liquid mixed reactor (10) also comprises:
Be arranged on kettle (11) outside, be connected to the first condensing unit (14) on the outlet port (111) of kettle (11), this first condensing unit (14) has: the exhaust outlet (141) being communicated with tail gas absorber (40), the steam inlet (142) being connected with the outlet port (111) of gas-liquid mixed reactor, the condensate liquid refluxing opening (143) being communicated with kettle (11).
3. reaction and the purification system of aliphatic as claimed in claim 2 or ring family diurethane, is characterized in that, the afterbody of this first condensing unit (14) is also provided with stop valve (144).
4. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, is characterized in that, the outside of described kettle (11) is also provided with heater (15).
5. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, is characterized in that, described paddle (121) is Double-layer oblique leaf turbine or six leaf disc turbines; Described paddle (121) is staggered and is arranged on shaft (122) with the first gas distributor (13).
6. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, it is characterized in that, described the first gas distributor (13) is the circular tube shaped thing of one end sealing, the tube wall of this first gas distributor (13) arranges some apertures, on every the first gas distributor (13) the summation of foraminate sectional area be more than or equal to the sectional area of this first gas distributor pipe caliber.
7. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, it is characterized in that, the outside of described luwa evaporator (20) is also provided with the second condensing unit (24) being connected with the top discharge mouth (22) of described luwa evaporator (20).
8. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, is characterized in that, described luwa evaporator (20) also comprises:
Be communicated with the light component gathering-device (25) of the outlet of the second condensing unit (24);
Be communicated with the heavy constituent receiving system (26) of luwa evaporator (20) bottom heavy constituent discharging opening (23).
9. reaction and the purification system of aliphatic as claimed in claim 1 or ring family diurethane, is characterized in that, described tail gas absorber (40) comprises:
Tower body (41), the middle part of this tower body (41) is filled with filler, and the bottom of this tower body (41) fills exhaust-gas treatment solution;
Be arranged on second gas distributor (42) of tower body bottom, this second gas distributor (42) is communicated with the outlet port (111) of gas-liquid mixed reactor (10);
Be arranged on the spray equipment (43) at tower body top, by circulating pump, the exhaust-gas treatment solution of locating of bottom, absorption tower be pumped into spray equipment.
10. a technique of preparing aliphatic or ring family diurethane, is characterized in that, this technique comprises following steps:
Step 1, by aliphatic/ring family diamines, urea, fatty alcohol and ionic liquid are with molar ratio computing 1:(1 ~ 5): (1 ~ 10): (1 ~ 6) is placed in gas-liquid mixed reactor (10), pass into nitrogen replacement air, reaction temperature is 150 DEG C ~ 350 DEG C, reaction pressure 0.5MPa ~ 3MPa, air inlet by reactor bottom passes into nitrogen, make the gas-liquid of raw material in kettle evenly mix and get rid of the accessory substance ammonia generating through the first gas distributor (13), reclaim through tail gas absorber (40), reaction time is 1 ~ 15h, one pot reaction is prepared aliphatic/ring family diurethane, wherein, described aliphatic/ring family diamines selects 1, 4-cyclohexane diamine, hexamethylene diamine, 4, 4'-diamino-dicyclohexyl methane, IPD, trimethyl hexamethylene diamine, any one in norbornane dimethylamine, described fatty alcohol is saturation unit fatty alcohol, described ionic liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-ethyl diethyldithiocarbamate ether-3-methyl imidazolium tetrafluoroborate, 1-ethyl acetate base-3-methylimidazole hexafluorophosphate, 1-butyl-2,3-methylimidazole bromine salt, tributyl octyl group bromide phosphine, 1-are fluoro-2, one or more combinations in 6-dichloropyridine tetrafluoroborate, 1-butyl-3-picoline tetrafluoroborate, 4-ethyl-4-methyl morpholine bromine salt, 1-ethyl-3-methylimidazole bis trifluoromethyl sulfimide salt,
Step 2, is transferred to the product of step 1 in luwa evaporator (20) by pump (30), separating-purifying light component and heavy constituent, and this light component refers to fatty alcohol solvent; This heavy constituent refers to aliphatic or ring family's diurethane and ionic liquid.
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| CN117326982A (en) * | 2022-09-30 | 2024-01-02 | 四川元理材料科技有限公司 | Industrial process for synthesizing isophorone dicarbamic acid n-butyl ester by urea method |
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| CN113694837A (en) * | 2020-05-21 | 2021-11-26 | 中国石油化工股份有限公司 | Kettle type reactor and method for unsaturated polymer hydrogenation and nitrile rubber hydrogenation method |
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| CN115403484A (en) * | 2022-09-30 | 2022-11-29 | 四川元理材料科技有限公司 | Industrial process for synthesizing isophorone diamino n-butyl formate by urea method |
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