CN106588650A - Method and system for feeding acetone cyanohydrin during preparation of methyl methacrylate - Google Patents
Method and system for feeding acetone cyanohydrin during preparation of methyl methacrylate Download PDFInfo
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- CN106588650A CN106588650A CN201611001177.9A CN201611001177A CN106588650A CN 106588650 A CN106588650 A CN 106588650A CN 201611001177 A CN201611001177 A CN 201611001177A CN 106588650 A CN106588650 A CN 106588650A
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- amide
- hydroxyisobutyronitrile
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/18—Preparation of carboxylic acid esters by conversion of a group containing nitrogen into an ester group
- C07C67/20—Preparation of carboxylic acid esters by conversion of a group containing nitrogen into an ester group from amides or lactams
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Abstract
The invention discloses a method for feeding acetone cyanohydrin during preparation of methyl methacrylate. The method comprises a step of jetting acetone cyanohydrin into an amide circulation loop, wherein the amide circulation loop is composed of an amide cooler, a gas separator and an amide circulation pump which is located between the outlet of the gas separator and the inlet of the amide cooler. According to the invention, through jetting of acetone cyanohydrin into the amide circulation loop at a plurality of positions, smaller acetone cyanohydrin drops are formed, so material mixing is more sufficient and faster, the decomposition degree of acetone cyanohydrin is reduced, the conversion rate of amide is increased, and unnecessary consumption of acetone cyanohydrin is lowered; thus, the conversion rate of an acylation reaction is increased.
Description
Technical field
The present invention relates to chemical field, and especially, the feed being related in a kind of methyl methacrylate preparation process
Method and system.
Background technology
Methyl methacrylate (referred to as MMA) is a kind of important Organic Chemicals and chemical products, is mainly used in
Production lucite (referred to as PMMA), polrvinyl chloride auxiliary agent A CR, copolymer of methyl methacrylate-styrene-butadiene
(referred to as MBS) and the second comonomer as acrylic fiber production process, it is also possible to make resin, adhesive, coating, ion exchange resin, paper
Open glazing agent, textile auxiliary, leather treatment, lube oil additive, pour point depressant for crude oil, the infiltration of timber and soft wood
Plasticizer of agent, the penetrant of motor coil, insulating potting material and shaped plastics emulsion etc., purposes is quite varied.
At present, in the world the main MMA production technologies for adopting include .alpha.-hydroxyisobutyronitrile. (ACH) method, isobutene. method and ethylene
Method.Wherein, most manufacturers (for example, being distributed mainly on North America and West Europe) adopt .alpha.-hydroxyisobutyronitrile. (ACH) method when MMA is produced,
And Japan mainly adopts the technique with isobutene. as raw material.In ethylene is adopted for the production technology of raw material MMA, work has been realized
Industry mainly has BASF technique and color spy (Lucite) company Alpha techniques of Britain fine jade.
The process characteristic of ACH methods is to be effectively utilized acrylonitrile installation by-product hydrocyanic acid, and MMA high incomes.ACH methods Jing
Cross and constantly improve for a long time and perfect, technology is relatively advanced, mature and reliable, good product quality, therefore has obtained widely used,
Jing becomes the dominating process route of current MMA productions.
First it is to carry out .alpha.-hydroxyisobutyronitrile. and sulphuric acid to be acylated instead in the technical process that MMA is produced by Acetone cyanohydrin method
Should, reaction generates α-formamido isopropyl hydrogen sulfuric acid ester.But, in currently used preparation facilitiess .alpha.-hydroxyisobutyronitrile. is adopted
Injection pipeline is directly injected into the mode of amide reactor and feeds, thus cause the mixing of .alpha.-hydroxyisobutyronitrile. and sulphuric acid not enough fully and
Rapidly, larger .alpha.-hydroxyisobutyronitrile. drop produces.So not only result in droplet surface and superheating phenomenon occur, cause part acetone
Cyanalcohol decomposes, and .alpha.-hydroxyisobutyronitrile. consumption can be caused to increase, and can reduce the conversion ratio of acylation reaction.
For the problems referred to above present in correlation technique, effective solution is not yet proposed at present.
The content of the invention
For the problems referred to above in correlation technique, the present invention proposes one kind and enters in methyl methacrylate preparation process
The feeding method of material .alpha.-hydroxyisobutyronitrile..The method can improve the conversion ratio of acylation reaction, and reduce the consumption of .alpha.-hydroxyisobutyronitrile..
The invention provides fed with acetone cyanogen in a kind of amide loop in methyl methacrylate preparation technology
The feeding system of alcohol.The feeding system includes amide cooler, gas trap and amide circulating pump, wherein amide circulating pump position
Between the outlet of gas trap and the entrance of amide cooler.The feeding system can have the positioned at first position
One .alpha.-hydroxyisobutyronitrile. blender, in the second .alpha.-hydroxyisobutyronitrile. ejector and tri acetylacetonate cyanalcohol ejector of second position extremely
It is few one.Wherein described first position is between the outlet of the amide cooler and the entrance of the gas trap the
Two positions are that between the gas trap and the amide circulating pump, tri acetylacetonate cyanalcohol ejector is separated positioned at the gas
In device.
In one embodiment, the feeding system can not have tri acetylacetonate cyanalcohol ejector, only with the one the third
At least one of ketone cyanalcohol blender and the second .alpha.-hydroxyisobutyronitrile. ejector.
In one embodiment, also have between the second .alpha.-hydroxyisobutyronitrile. ejector and amide circulating pump gas trap
Sulphuric acid blender.The sulphuric acid blender is used to inject sulphuric acid after injection .alpha.-hydroxyisobutyronitrile..In another embodiment, second
.alpha.-hydroxyisobutyronitrile. ejector can be exchanged with the position of sulphuric acid blender, i.e. sulphuric acid blender is by sulphuric acid from positioned at the second acetone cyanogen
Between alcohol ejector and the outlet of gas trap in position injection amide closed circuit.Second .alpha.-hydroxyisobutyronitrile. ejector and sulphuric acid
After blender transposition, sulphuric acid blender can inject sulphuric acid before injection .alpha.-hydroxyisobutyronitrile..In one embodiment, the sulfur
Sour blender is sulphuric acid static mixer.
Present invention also offers a kind of amide loop being fed to .alpha.-hydroxyisobutyronitrile. in methyl methacrylate preparation technology
In feeding method.The method includes .alpha.-hydroxyisobutyronitrile. being injected in the amide closed circuit in the way of spraying.
In one embodiment, by the first .alpha.-hydroxyisobutyronitrile. blender positioned at first position and positioned at second position
At least one of the second .alpha.-hydroxyisobutyronitrile. ejector injecting .alpha.-hydroxyisobutyronitrile..Described first position is the amide cooler
Outlet and the entrance of the gas trap between, the second position be the gas trap and the amide circulating pump it
Between.In a kind of specific embodiment, be with the weight ratio of the .alpha.-hydroxyisobutyronitrile. injection rate of the second position in first position (1～
3)：1, preferably 2:1.
In one embodiment, by positioned at first position the first .alpha.-hydroxyisobutyronitrile. blender, positioned at second position
The second .alpha.-hydroxyisobutyronitrile. ejector and at least one of tri acetylacetonate cyanalcohol ejector injection .alpha.-hydroxyisobutyronitrile..A kind of specific
In embodiment, the weight ratio of the .alpha.-hydroxyisobutyronitrile. injection rate of the first position, the second position and the 3rd position is
(1～3)：1：1, preferably 2:1:1.
In one embodiment, described feed process is further included sulphuric acid by sulphuric acid static mixer from
In position injection amide closed circuit between two .alpha.-hydroxyisobutyronitrile. ejectors and the entrance of amide circulating pump.After sulphuric acid injection,
Injection .alpha.-hydroxyisobutyronitrile..It is to meet chemical process equipment for sulphuric acid injection does not have specific restriction with the speed of three ACH injections
Specified in permissible velocity.In a kind of specific embodiment, the .alpha.-hydroxyisobutyronitrile. total amount injected in amide closed circuit
It is (1.5～1.6) with the mol ratio of sulphuric acid：1.
In a kind of embodiment of described feed process of the present invention, the temperature of amide closed circuit is maintained at
85 DEG C～95 DEG C, and the pressure of the amide closed circuit is maintained at into 0.01～0.05MPaG.
The present invention is the multiple positions in amide closed circuit injecting .alpha.-hydroxyisobutyronitrile. by way of spraying, enabling
Less .alpha.-hydroxyisobutyronitrile. drop is formed, so that material mixes more fully and quick, the degree of decomposition of .alpha.-hydroxyisobutyronitrile. is reduced,
The conversion ratio of amide is improve, while reducing the unnecessary consumption of .alpha.-hydroxyisobutyronitrile., the efficiency of acylation reaction is improved.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to institute in embodiment
The accompanying drawing that needs are used is briefly described, it should be apparent that, drawings in the following description are only some enforcements of the present invention
Example, for those of ordinary skill in the art, on the premise of not paying creative work, can be being obtained according to these accompanying drawings
Obtain other accompanying drawings.
Fig. 1 is the signal for preparing the amide closed circuit structure of methyl methacrylate according to embodiments of the present invention
Figure.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.Hereinafter implement
Example is not limited to the scope of the present invention for illustrating the present invention.
A kind of embodiments in accordance with the present invention, there is provided the feed side of .alpha.-hydroxyisobutyronitrile. in methyl methacrylate preparation process
Method.The method can improve Acetone cyanohydrin method production methyl methacrylate amidation process conversion ratio, and reduce .alpha.-hydroxyisobutyronitrile.
Consumption.
Method of the present invention includes：.alpha.-hydroxyisobutyronitrile. is injected in amide closed circuit in the way of spraying, wherein,
Constituting the equipment of amide closed circuit includes amide cooler, gas trap and amide circulating pump, and amide circulating pump is located at
Between the outlet of gas trap and the entrance of amide cooler.
In one embodiment, the position for injecting .alpha.-hydroxyisobutyronitrile. with spray regime includes at least one of：First
Put, between the outlet of amide cooler and the entrance of gas trap；Second injection phase, positioned at gas trap and acyl
Between amine circulating pump.In this case, the weight ratio of the .alpha.-hydroxyisobutyronitrile. injection rate of first position and second position for (1～
3)：1.Fig. 1 shows amide closed circuit, including amide circulating pump P-1, amide cooler E-1 and gas trap
V-1.In the present embodiment, the first .alpha.-hydroxyisobutyronitrile. blender M-1 is located at first position, and the second .alpha.-hydroxyisobutyronitrile. ejector J-1 is located at
The second position, and sulphuric acid blender M-2 can be arranged between the second .alpha.-hydroxyisobutyronitrile. ejector J-1 and amide circulating pump P-1.
In another embodiment, the position for injecting .alpha.-hydroxyisobutyronitrile. with spray regime includes at least one of：First position,
Between the outlet of amide cooler and gas trap；The second position, between gas trap and amide circulating pump；
3rd position, in gas trap.Now, the acetone cyanogen for injecting at first position, the second position and the 3rd position
The weight ratio of the amount of alcohol is (1～3)：1：1.Referring also to Fig. 1, in the present embodiment, the first .alpha.-hydroxyisobutyronitrile. blender M-1 is located at the
One position, the second .alpha.-hydroxyisobutyronitrile. ejector J-1 can be arranged on (second between gas trap V-1 and amide circulating pump P-1
Put).In order that the droplet size being injected in four-way, acquisition preferably effect can be done before amide circulating pump using ejector
Really.Tri acetylacetonate cyanalcohol ejector (not shown) can be arranged at gas trap V-1 (the 3rd position), so as to directly to gas
Injection injection .alpha.-hydroxyisobutyronitrile. in separator V-1.By using the first .alpha.-hydroxyisobutyronitrile. blender and the second .alpha.-hydroxyisobutyronitrile. ejector
The combination of (and/or tri acetylacetonate cyanalcohol ejector), the injection in loop that can be realized has various sizes of drop, in acyl
Before amine circulating pump using .alpha.-hydroxyisobutyronitrile. jet effect more preferably.Material enters amide by gravity from the outlet of gas trap
Circulating pump, pumps into amide cooler, so as to realize the circulation of material Jing after the boosting of amide circulating pump by material.
Additionally, the method may further include：Sulphuric acid is circulated from gas trap and amide by sulphuric acid blender
In position injection amide closed circuit between pump.Referring to Fig. 1, sulphuric acid blender M-2 can be arranged on gas trap V-1 with
Between the import of amide circulating pump P-1.
Alternatively, the mol ratio of the .alpha.-hydroxyisobutyronitrile. total amount and sulphuric acid of injecting amide closed circuit is (1.5～1.6)：1, it is excellent
Elect 1.5 as：1.
Additionally, the method may further include：The temperature of amide closed circuit is maintained at into 85 DEG C～95 DEG C, by pressure
It is maintained at 0.01～0.05MPaG.
According to the embodiment of the present invention, additionally provide a kind of .alpha.-hydroxyisobutyronitrile. for preparing methyl methacrylate to be fed
System.Multiple positions injection .alpha.-hydroxyisobutyronitrile. that the system is used in amide closed circuit, wherein, constitute amide closed circuit
Equipment include amide cooler (referring to the amide cooler E-1 in Fig. 1, can by way of water-cooled, with recirculated water supply water and
Recirculated water backwater connect), gas trap (referring to the gas trap V-1 in Fig. 1, can be further attached to amide heating
Device) and amide circulating pump (referring to the amide circulating pump P-1 in Fig. 1), amide circulating pump be located at the outlet of gas trap with
Between the entrance of amide cooler, the feeding system includes：
First .alpha.-hydroxyisobutyronitrile. blender (such as the .alpha.-hydroxyisobutyronitrile. blender M-1 in Fig. 1), is arranged on going out for amide cooler
Between mouth and gas trap (that is, first position)；
Second .alpha.-hydroxyisobutyronitrile. ejector (not shown), is arranged between gas trap and amide circulating pump (that is, above-mentioned
Two injection phases)；
Wherein, the second .alpha.-hydroxyisobutyronitrile. ejector can be continuously injected into .alpha.-hydroxyisobutyronitrile. in the way of spraying.
Additionally, the system may further include：
Tri acetylacetonate cyanalcohol ejector (not shown), is arranged in gas trap (that is, above-mentioned 3rd position), for
The mode of injection is directly injected into .alpha.-hydroxyisobutyronitrile. in gas trap.
Each specific embodiment of the present invention is described more fully below.
Embodiment 1
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at two positions
It is divided to two strands to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein one .alpha.-hydroxyisobutyronitrile. is by the first .alpha.-hydroxyisobutyronitrile. positioned at first position
Blender M-1 is continuously added in amide closed circuit, and another strand of .alpha.-hydroxyisobutyronitrile. is connected by the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being ejected into amide closed circuit continuously.Wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 be arranged on the outlet of amide cooler E1 with
On pipeline between the entrance of gas trap V1.By the .alpha.-hydroxyisobutyronitrile. of the first .alpha.-hydroxyisobutyronitrile. blender M-1 and by second
The weight ratio of the .alpha.-hydroxyisobutyronitrile. of .alpha.-hydroxyisobutyronitrile. ejector J-1 injections is 3:1.The concentrated sulphuric acid and acetone cyanogen being injected in amide loop
The mol ratio of alcohol total amount is 1.6:1.Operation is carried out at a temperature of 89 DEG C and under the pressure of 0.05MPaG.
Concentrated sulphuric acid reacts rapidly after mixing with .alpha.-hydroxyisobutyronitrile., generates intermediate methyl acrylic acid amides sulfate,
Obtain amide blend.In amide closed circuit, amide circulating pump P-1 extracts acyl from the bottom of first gas separator V-1
Amine blends, make amide blend order by the second .alpha.-hydroxyisobutyronitrile. ejector J1, sulphuric acid blender M-2, amide circulating pump, acyl
Amine cooler E-1, the first .alpha.-hydroxyisobutyronitrile. blender M-1, return to first gas separator V-1, form closed circuit.Wherein material
Amide circulating pump is entered from gas trap by gravity, and circulation can be maintained Jing after the boosting of amide circulating pump.In the step reaction
Reaction heat in amide cooler E-1 by circulation cooling water remove.Being capable of shape by the injection of multipoint mode .alpha.-hydroxyisobutyronitrile.
The .alpha.-hydroxyisobutyronitrile. drop of Cheng Geng little, and amide circulating pump suction line sprayed feed material is mixed it is more fully and fast
Speed, these factors significantly reduce the degree of decomposition of ACH.Consumption of raw materials is reduced by using the system of embodiment 1, acyl is made
The conversion ratio for changing reaction improves 0.2%.
Embodiment 2
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at two positions
It is divided to two strands to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein one .alpha.-hydroxyisobutyronitrile. is by the first .alpha.-hydroxyisobutyronitrile. positioned at first position
Blender M-1 is continuously added in amide closed circuit, and another strand of .alpha.-hydroxyisobutyronitrile. is connected by the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being ejected into amide closed circuit continuously.Wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 is arranged on outlet and the gas of amide cooler
On pipeline between the entrance of body separator.By the .alpha.-hydroxyisobutyronitrile. of the first .alpha.-hydroxyisobutyronitrile. blender M-1 and by the second acetone
The weight ratio of the .alpha.-hydroxyisobutyronitrile. of cyanalcohol ejector J-1 injections is 1:1.The concentrated sulphuric acid being injected in amide loop is total with .alpha.-hydroxyisobutyronitrile.
The mol ratio of amount is 1.5:1.Operation is carried out at a temperature of 85 DEG C and under the pressure of 0.01MPaG.
By reducing consumption of raw materials using the system of embodiment 2, the conversion ratio for acidylating reaction improves 0.1%.
Embodiment 3
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at two positions
It is divided to two strands to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein one .alpha.-hydroxyisobutyronitrile. is by the first .alpha.-hydroxyisobutyronitrile. positioned at first position
Blender M-1 is continuously added in amide closed circuit, and another strand of .alpha.-hydroxyisobutyronitrile. is connected by the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being ejected into amide closed circuit continuously.Wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 is arranged on the outlet in amide cooler E-1
And on the pipeline between the entrance of gas trap V1.By the .alpha.-hydroxyisobutyronitrile. of the first .alpha.-hydroxyisobutyronitrile. blender M-1 and by
The weight ratio of the .alpha.-hydroxyisobutyronitrile. of two .alpha.-hydroxyisobutyronitrile. ejector J1 injections is 2:1.The concentrated sulphuric acid and acetone being injected in amide loop
The mol ratio of cyanalcohol total amount is 1.5:1.Operation is carried out at a temperature of 87 DEG C and under the pressure of 0.03MPaG.
Consumption of raw materials is reduced by the system of practical embodiment 3, the conversion ratio for acidylating reaction improves 0.25%.
Embodiment 4
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at two positions
It is divided to two strands to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein one .alpha.-hydroxyisobutyronitrile. is by the first .alpha.-hydroxyisobutyronitrile. positioned at first position
Blender M-1 is continuously added in amide closed circuit, and another strand of .alpha.-hydroxyisobutyronitrile. is connected by the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being ejected into amide closed circuit continuously.Wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 is arranged on the outlet in amide cooler E-1
And on the pipeline between the entrance of gas trap V-1.By the .alpha.-hydroxyisobutyronitrile. of the first .alpha.-hydroxyisobutyronitrile. blender M-1 and by
The weight ratio of the .alpha.-hydroxyisobutyronitrile. of two .alpha.-hydroxyisobutyronitrile. ejector J-1 injections is 1:1.The concentrated sulphuric acid and acetone being injected in amide loop
The mol ratio of cyanalcohol total amount is 1.6:1.Operation is carried out at a temperature of 90 DEG C and under the pressure of 0.05MPaG.
Consumption of raw materials is reduced by using the system of embodiment 4, the conversion ratio for acidylating reaction improves 0.1%.
Embodiment 5
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at two positions
It is divided to two strands to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein one .alpha.-hydroxyisobutyronitrile. is by the first .alpha.-hydroxyisobutyronitrile. positioned at first position
Blender M-1 is continuously added in amide closed circuit, and another strand of .alpha.-hydroxyisobutyronitrile. is connected by the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being ejected into amide closed circuit continuously.Wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 is arranged on the outlet in amide cooler E-1
On the pipeline of the entrance of gas trap V-1.By the .alpha.-hydroxyisobutyronitrile. of the first .alpha.-hydroxyisobutyronitrile. blender M-1 and by the two the third
The weight ratio of the .alpha.-hydroxyisobutyronitrile. of ketone cyanalcohol ejector J-1 injections is 2:1.The concentrated sulphuric acid and .alpha.-hydroxyisobutyronitrile. being injected in amide loop
The mol ratio of total amount is 1.55:1.Operation is carried out at a temperature of 88 DEG C and under the pressure of 0.04MPaG.
Consumption of raw materials is reduced by using the system of embodiment 5, the conversion ratio for acidylating reaction improves 0.2%.
Embodiment 6
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at three positions
Three strands are divided to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein first strand of .alpha.-hydroxyisobutyronitrile. is by the first acetone cyanogen positioned at first position
Alcohol blender M-1 is continuously added in amide closed circuit, and second strand of .alpha.-hydroxyisobutyronitrile. passes through the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being continuously ejected into amide closed circuit, the 3rd strand of .alpha.-hydroxyisobutyronitrile. is by the tri acetylacetonate cyanalcohol spray in gas trap
Emitter (not shown) is continuously ejected in amide closed circuit.It is cold that wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 is arranged on amide
But on the pipeline between the E-1 outlets of device and the entrance of gas trap V-1.By the acetone of the first .alpha.-hydroxyisobutyronitrile. blender M1
Cyanalcohol, by the second .alpha.-hydroxyisobutyronitrile. ejector J-1 inject .alpha.-hydroxyisobutyronitrile. and by tri acetylacetonate cyanalcohol ejector inject third
The weight ratio of ketone cyanalcohol is 3:1：1.The concentrated sulphuric acid being injected in amide loop is 1.55 with the mol ratio of .alpha.-hydroxyisobutyronitrile. total amount:1.
Operation is carried out at a temperature of 90 DEG C and under the pressure of 0.05MPaG.
Consumption of raw materials is reduced by using the system of embodiment 6, the conversion ratio for acidylating reaction improves 0.3%.
Embodiment 7
Concentrated sulphuric acid is continuously added in amide closed circuit by sulphuric acid blender M-2.Afterwards at three positions
Three strands are divided to inject .alpha.-hydroxyisobutyronitrile. with spray regime, wherein first strand of .alpha.-hydroxyisobutyronitrile. is by the first acetone cyanogen positioned at first position
Alcohol blender M-1 is continuously added in amide closed circuit, and second strand of .alpha.-hydroxyisobutyronitrile. passes through the second .alpha.-hydroxyisobutyronitrile. ejector J-1
In being continuously ejected into amide closed circuit, the 3rd strand of .alpha.-hydroxyisobutyronitrile. is by the tri acetylacetonate cyanalcohol spray in gas trap
Emitter (not shown) is continuously ejected in amide closed circuit.It is cold that wherein the first .alpha.-hydroxyisobutyronitrile. blender M-1 is arranged on amide
But on the pipeline between the entrance of the outlet of device E-1 and gas trap V-1.Injected by the first .alpha.-hydroxyisobutyronitrile. blender M-1
.alpha.-hydroxyisobutyronitrile., by the second .alpha.-hydroxyisobutyronitrile. ejector J-1 inject .alpha.-hydroxyisobutyronitrile. and by tri acetylacetonate cyanalcohol ejector note
The weight ratio of the .alpha.-hydroxyisobutyronitrile. for entering is 1:1:1.The concentrated sulphuric acid being injected in amide loop is with the mol ratio of .alpha.-hydroxyisobutyronitrile. total amount
1.5:1.Aforesaid operations are carried out at a temperature of 95 DEG C and under the pressure of 0.01MPaG.
Consumption of raw materials is reduced by using the system of embodiment 7, the conversion ratio for acidylating reaction improves 0.09%.
Comparative example 1(.alpha.-hydroxyisobutyronitrile., i.e. second position are only added at a position)
In comparative example 1 .alpha.-hydroxyisobutyronitrile. blender is located between the import of amide cooler and amide circulating pump, in acetone
There is sulphuric acid blender between cyanalcohol ejector and gas trap.Concentrated sulphuric acid is continuously added by acyl by sulphuric acid gaseous mixture
In amine closed circuit.Afterwards .alpha.-hydroxyisobutyronitrile. is added in amide closed circuit by .alpha.-hydroxyisobutyronitrile. blender.Wherein sulphuric acid is mixed
Clutch and .alpha.-hydroxyisobutyronitrile. blender are arranged on the pipeline between the import of amide cooler and amide circulating pump.It is injected into acyl
Concentrated sulphuric acid in amine loop is 1.5 with the mol ratio of .alpha.-hydroxyisobutyronitrile.:1.Operation at a temperature of 90 DEG C and 0.05MPaG pressure
Carry out under power.
Comparative example 2(.alpha.-hydroxyisobutyronitrile. being added at three positions, using non-ejection mode)
In comparative example 2 .alpha.-hydroxyisobutyronitrile. blender is located between the import of amide cooler and amide circulating pump, in acetone
There is sulphuric acid blender between cyanalcohol ejector and gas trap.Afterwards two strands of addition .alpha.-hydroxyisobutyronitrile .s are punished two positions,
Wherein one .alpha.-hydroxyisobutyronitrile. is continuously injected into amide looping back by the first .alpha.-hydroxyisobutyronitrile. blender positioned at first position
Lu Zhong, second strand of .alpha.-hydroxyisobutyronitrile. is continuously injected in amide closed circuit by the second .alpha.-hydroxyisobutyronitrile. blender, the 3rd strand third
Ketone cyanalcohol is continuously ejected into amide and loops back by the tri acetylacetonate cyanalcohol ejector (not shown) in gas trap
Lu Zhong..Wherein the first .alpha.-hydroxyisobutyronitrile. blender is arranged on the outlet of amide cooler E-1 and the entrance of gas trap V-1
On pipeline.By the .alpha.-hydroxyisobutyronitrile. of the first .alpha.-hydroxyisobutyronitrile. blender, the .alpha.-hydroxyisobutyronitrile. injected by the second .alpha.-hydroxyisobutyronitrile. blender
It is 3 with the weight ratio of the .alpha.-hydroxyisobutyronitrile. of tri acetylacetonate cyanalcohol blender injection:1:1.Be injected into concentrated sulphuric acid in amide loop with
The mol ratio of .alpha.-hydroxyisobutyronitrile. total amount is 1.5:1.Operation is carried out at a temperature of 90 DEG C and under the pressure of 0.05MPaG.
Table 1
As shown in above-mentioned embodiment, by multiple positions in amide closed circuit spraying in embodiment 1-7
Mode injects .alpha.-hydroxyisobutyronitrile. so that the conversion ratio of amide improves more than 0.1%.In embodiment 6, amide conversion ratio improves
0.3%, while the consumption of .alpha.-hydroxyisobutyronitrile. is reduced.Comparatively, comparative example 1 is the method generally adopted in prior art, wherein
Heretofore described .alpha.-hydroxyisobutyronitrile. ejector is not used .alpha.-hydroxyisobutyronitrile. is to be added to amide loop in disposable mode
In..alpha.-hydroxyisobutyronitrile. is added in three various locations in comparative example 2, but is provided without non-ejection mode and added.From the knot of comparative example 2
From the point of view of fruit, the conversion ratio of amide reaction also makes moderate progress, but the amplitude for improving is less.From above-described embodiment and the result of comparative example
, it can be seen that .alpha.-hydroxyisobutyronitrile. is injected in the way of spraying in multiple positions in amide loop, less .alpha.-hydroxyisobutyronitrile. can be formed
Drop, so that material mixes more fully and quick..alpha.-hydroxyisobutyronitrile. is added using this sample loading mode, dividing for .alpha.-hydroxyisobutyronitrile. is reduced
Solution degree, improves the conversion ratio of amide.Meanwhile, being added with spray regime can reduce the unnecessary consumption of .alpha.-hydroxyisobutyronitrile., improve
The efficiency of acylation reaction.
In sum, by means of technical scheme .alpha.-hydroxyisobutyronitrile. in circulating reaction system is acylated to MMA devices
Charging points and every injection rate are optimized and calculate, by the injection injection and flow-control of multipoint mode .alpha.-hydroxyisobutyronitrile.,
Less .alpha.-hydroxyisobutyronitrile. drop can be formed, the unnecessary consumption of .alpha.-hydroxyisobutyronitrile. is reduced, the conversion ratio of acylation reaction is improved, is made
Obtain material and mix more fully and quick, reduce the degree of decomposition of .alpha.-hydroxyisobutyronitrile. so that the conversion ratio of amide improves about
More than 0.1%, improve about 0.2%, about 0.25%, or even improve about 0.3% or higher.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Within god and principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.
Claims (11)
1. in a kind of amide loop in methyl methacrylate preparation technology fed with acetone cyanalcohol feeding system, its
It is characterised by, the feeding system includes amide cooler, gas trap and amide circulating pump, the amide circulating pump is located at
Between the outlet of the gas trap and the entrance of the amide cooler, the feeding system has positioned at first position
First .alpha.-hydroxyisobutyronitrile. blender, in the second .alpha.-hydroxyisobutyronitrile. ejector and tri acetylacetonate cyanalcohol ejector of second position
At least one, the first position is between the outlet of the amide cooler and the import of the gas trap described the
Two positions are that between the gas trap and the amide circulating pump, the tri acetylacetonate cyanalcohol ejector is located at the gas
In separator.
2. feeding system according to claim 1, it is characterised in that the feeding system mixes with the first .alpha.-hydroxyisobutyronitrile.
At least one of device and the second .alpha.-hydroxyisobutyronitrile. ejector.
3. feeding system according to claim 1 and 2, it is characterised in that in the second .alpha.-hydroxyisobutyronitrile. ejector and institute
State and also have between amide circulating pump gas trap sulphuric acid blender.
4. the feeding method in a kind of amide loop that .alpha.-hydroxyisobutyronitrile. is fed in methyl methacrylate preparation technology, it is special
Levy and be, methods described includes：.alpha.-hydroxyisobutyronitrile. is injected in the amide closed circuit in the way of spraying, wherein, it is described
Feeding system includes amide cooler, gas trap and amide circulating pump, and the amide circulating pump is separated positioned at the gas
Between the outlet of device and the entrance of the amide cooler.
5. feeding method according to claim 4, it is characterised in that mixed by the first .alpha.-hydroxyisobutyronitrile. positioned at first position
At least one of clutch and the second .alpha.-hydroxyisobutyronitrile. ejector positioned at second position to inject .alpha.-hydroxyisobutyronitrile., described first
It is set between the outlet of the amide cooler and the entrance of the gas trap, the second position is gas separation
Between device and the amide circulating pump.
6. feeding method according to claim 5, it is characterised in that in the first position and the third of the second position
The weight ratio of ketone cyanalcohol injection rate is (1～3)：1.
7. feeding method according to claim 4, it is characterised in that
By positioned at the first .alpha.-hydroxyisobutyronitrile. blender of first position, the second .alpha.-hydroxyisobutyronitrile. ejector positioned at second position and
At least one of tri acetylacetonate cyanalcohol ejector injects .alpha.-hydroxyisobutyronitrile., and the first position is the outlet of the amide cooler
And the entrance of the gas trap between, the second position is the outlet of the gas trap and the amide circulating pump
Entrance between, the tri acetylacetonate cyanalcohol ejector be located at the gas trap in.
8. feeding method according to claim 7, it is characterised in that the first position, the second position and described
The weight ratio of the .alpha.-hydroxyisobutyronitrile. injection rate of the 3rd position is (1～3)：1：1.
9. feeding method according to claim 4, it is characterised in that further include：
By sulphuric acid blender by sulphuric acid from the entrance positioned at the second .alpha.-hydroxyisobutyronitrile. ejector and the amide circulating pump it
Between position inject in the amide closed circuit, or the sulphuric acid blender by sulphuric acid from spraying positioned at second .alpha.-hydroxyisobutyronitrile.
Position is injected in the amide closed circuit between the outlet of emitter and the gas trap.
10. feeding method according to claim 9, it is characterised in that the .alpha.-hydroxyisobutyronitrile. of the injection amide closed circuit
Total amount is (1.5～1.6) with the mol ratio of sulphuric acid：1.
11. feeding methods according to any one of claim 4-10, it is characterised in that
The temperature of the amide closed circuit is maintained at into 85 DEG C～95 DEG C, and the pressure of the amide closed circuit is maintained at
0.01～0.05MPaG.
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