Production device of N-methylguanidinoacetic acid

Abstract

The utility model relates to the technical field of chemical equipment, in particular to a production device of N-methylguanidinoacetic acid. According to the technical scheme, the device comprises a dissolving kettle, a mother liquor kettle, a tubular reactor, a pH adjusting kettle, a concentration kettle, a crystallization kettle and a rotary furnace, a dissolving constant-temperature heat exchanger is arranged on the outer wall of the dissolving kettle, and a dissolving liquid outlet is formed in the bottom of the dissolving kettle and connected with reaction inlets of the mother liquor kettle and the tubular reactor; a mother liquid outlet is formed in the bottom of the mother liquid kettle, a mother liquid constant-temperature heat exchanger is arranged on the outer wall, and a top mother liquid inlet is communicated with a concentrated liquid outlet in the bottom of the concentration kettle; a reaction constant-temperature heat exchanger is sleeved on the outer wall of the tubular reactor, and a reaction outlet is formed to be communicated with a top pH adjusting feeding hole of the pH adjusting kettle. The high-purity N-methylguanidinoacetic acid monohydrate is continuously produced in a continuous feeding and intermittent discharging mode, and the equipment utilization rate and the production efficiency are improved.

Description

Technical Field

[0001] This utility model relates to the field of chemical equipment technology, and in particular to a production apparatus for N-methylguanidinoacetic acid. Background Technology

[0002] N-Methylguanidinoacetic acid, also known as creatine, with the chemical formula C4H9N3O2, is a nitrogen-containing organic acid. It naturally exists in vertebrates and helps provide energy to muscle and nerve cells, accelerating muscle strength and fatigue recovery. In recent years, creatine monohydrate, as the main product form of creatine, has been widely used in food, pharmaceuticals, and health supplements, and is highly favored by middle-aged and elderly people, athletes, and fitness enthusiasts.

[0003] The traditional method for synthesizing N-methylguanidinoacetic acid involves first synthesizing crude creatine from aminocyanide and sarcosine salt, followed by purification. Traditional N-methylguanidinoacetic acid production equipment generates impurities such as dicyandiamide and dihydrotriazine during the production process, requiring complex purification treatments, increasing process steps, extending the production cycle, increasing costs, and hindering market competitiveness. To address this, this invention provides a production apparatus for N-methylguanidinoacetic acid. Summary of the Invention

[0004] To address the problems existing in the prior art, the present invention provides a production apparatus for N-methylguanidinoacetic acid, which uses a continuous feeding and intermittent discharge method to achieve continuous production of N-methylguanidinoacetic acid, while reducing raw material recovery costs and improving raw material utilization by suppressing side reactions.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] The present invention relates to a production apparatus for N-methylguanidinoacetic acid, characterized in that it includes a dissolving vessel, a mother liquor vessel, a tubular reactor, a pH adjusting vessel, a concentration vessel, a crystallization vessel, and a rotary furnace. The outer wall of the dissolving vessel is provided with a dissolving constant temperature heat exchanger, and the bottom is provided with a dissolving outlet that is connected to the reaction inlet of the mother liquor vessel and the tubular reactor through a first tee.

[0007] The bottom of the mother liquor tank is provided with a mother liquor outlet connected to a first three-way valve, the outer wall is provided with a mother liquor constant temperature heat exchanger, and the top mother liquor inlet is connected to the concentration outlet at the bottom of the concentration tank.

[0008] The outer wall of the tubular reactor is fitted with a reaction constant temperature heat exchanger, and a reaction outlet is provided that connects to the top pH adjustment inlet of the pH adjustment vessel; the top pH adjustment outlet of the pH adjustment vessel is connected to the concentration inlet of the concentration vessel and the crystallization inlet of the crystallization vessel through a second tee.

[0009] The bottom of the crystallization kettle is equipped with a crystallization outlet, which is connected to the rotary kiln and the crystallization water recovery pipeline via a third tee.

[0010] According to the production device of N-methyl guanidine acetic acid, the dissolving inlet of the dissolving kettle is connected with a first three-way joint, a transmission pump, an electronic flow meter and a valve in sequence through a pipeline.

[0011] According to the production device of N-methyl guanidine acetic acid, the mother liquor outlet of the mother liquor kettle is connected with a transmission pump, an electronic flow meter and a valve in sequence through a pipeline, and the electronic flow meter and the valve are connected with the transmission pump of the dissolving pipeline through a PLC to form a interlocking structure.

[0012] The top of the mother liquor kettle is provided with a mother liquor supplementing inlet, and the pipeline connected with the mother liquor supplementing inlet is connected with a valve, an electronic flow meter and a transmission pump in sequence.

[0013] According to the production device of N-methyl guanidine acetic acid, the top of the pH adjusting kettle is provided with a pH adjusting material inlet and a pH adjusting liquid inlet, the bottom is provided with a pH adjusting material outlet, and the outer wall is provided with a pH adjusting constant temperature heat exchanger, the pH adjusting material inlet is connected with the reaction outlet through a pipeline and connected with a valve, an electronic flow meter and a transmission pump in sequence, the pH adjusting liquid inlet is connected with a hydrochloric acid pipeline through a pipeline and connected with a valve, an electronic flow meter and a transmission pump in sequence, and the pH adjusting material outlet is connected with the concentration kettle and the crystallization kettle through a second three-way joint.

[0014] According to the production device of N-methyl guanidine acetic acid, the top of the concentration kettle is provided with a concentration liquid inlet and a concentration gas outlet, the bottom is provided with a concentration liquid outlet, and the outer wall is provided with a concentration constant temperature heat exchanger, the concentration gas outlet is connected with a recovered water storage tank through a pipeline and connected with a valve and a vacuum pump in sequence, and the concentration liquid outlet is connected with the mother liquor liquid inlet through a pipeline and connected with a valve, an electronic flow meter and a filtration pump in sequence.

[0015] According to the production device of N-methyl guanidine acetic acid, the top of the crystallization kettle is provided with a crystallization material inlet and a crystallization water inlet, the bottom is provided with a crystallization material outlet and a crystallization weighing module, and the outer wall is provided with a crystallization constant temperature heat exchanger, the crystallization water inlet is connected with a pure water pipeline through a pipeline and connected with a valve, an electronic flow meter and a transmission pump in sequence, and the crystallization material outlet is connected with a rotary furnace and a crystallization water recovery pipeline through a third three-way joint.

[0016] According to the production device of N-methyl guanidine acetic acid, the left end of the rotary furnace is provided with a rotary furnace inlet, and the right end is provided with a rotary furnace outlet, the rotary furnace outlet is connected with a product storage tank through a pipeline and connected with a valve in sequence.

[0017] According to the production device of N-methyl guanidine acetic acid, the dissolving kettle, the mother liquor kettle, the pH adjusting kettle, the concentration kettle and the crystallization kettle need to be parallel connected, and N≥2.

[0018] The production device of N-methyl guanidino acetic acid provided by the utility model continuously produces high-purity monohydrate N-methyl guanidino acetic acid through the mode of continuous feeding and intermittent discharging, improves equipment utilization rate and production efficiency, and reduces production cost;

[0019] The utility model discloses through the generation of inhibiting impurity dicyandiamide and further avoid the production of guanidino creatine, dihydrotriazine and other impurities, reduce product purification and raw material recovery difficulty, improve the utilization of raw material, reduce production cost. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 It is whole structure schematic diagram of the utility model

[0021] In the drawing: 1, dissolving kettle, 101, dissolving inlet, 102, dissolving outlet, 103, dissolving constant temperature heat exchanger, 2, mother liquor kettle, 201, mother liquor liquid supplementing port, 202, mother liquor inlet, 203, mother liquor outlet, 204, mother liquor constant temperature heat exchanger, 3, tubular reactor, 301, reaction inlet, 302, reaction outlet, 303, reaction constant temperature heat exchanger, 4, pH adjusting kettle, 401, pH adjusting feed port, 402, pH adjusting inlet, 403, pH adjusting outlet, 404, pH adjusting constant temperature heat exchanger, 5, concentration kettle, 501, concentration inlet, 502 concentration outlet, 503, concentration outlet, 504, concentration constant temperature heat exchanger, 6, crystallization kettle, 601, crystallization feed port, 602, crystallization water inlet, 603, crystallization outlet, 604, crystallization weighing module, 605, crystallization constant temperature heat exchanger, 7, rotary furnace, 701, converter inlet, 702, converter outlet, 8, PLC interlocking device, 9, first tee, 10, second tee, 11, third tee. DETAILED DESCRIPTION

[0022] The utility model makes further detailed description in combination with the drawings and specific embodiment.

[0023] The utility model discloses dissolving kettle 1, mother liquor kettle 2, tubular reactor 3, pH adjusting kettle 4, concentration kettle 5, crystallization kettle 6 and rotary furnace 7, the top of dissolving kettle 1 is equipped with inlet 101, is equipped with outlet 102 in the bottom, is equipped with constant temperature heat exchanger 103 on the outer wall, dissolving inlet 101 is connected sodium creatine dissolving kettle through the pipeline and is connected valve, electronic flowmeter and transmission pump in series, dissolving outlet 102 is connected mother liquor kettle 2 and tubular reactor 3 through first tee 9.

[0024] The top of mother liquor kettle 2 is equipped with mother liquor water inlet 201 and mother liquor inlet 202, is equipped with mother liquor outlet 203 in the bottom, is equipped with constant temperature heat exchanger 204 on the outer wall, mother liquor water inlet 201 is connected pure water pipeline through the pipeline and is connected valve, electronic flowmeter and transmission pump in series.

[0025] The tubular reactor 3 is provided with a reaction inlet 301 at one end and a reaction outlet 302 at the other end, and the outer wall is sleeved with a reaction constant-temperature heat exchanger 303.

[0026] The top of the pH adjusting kettle 4 is provided with a pH adjusting feed inlet 401 and a pH adjusting liquid inlet 402, the bottom is provided with a pH adjusting discharge outlet 403, the outer wall is provided with a pH adjusting constant-temperature heat exchanger 404, the pH adjusting feed inlet 401 is connected to the reaction outlet 302 through a pipeline and connected in series with a valve, an electronic flowmeter and a transfer pump, the pH adjusting liquid inlet 402 is connected to a hydrochloric acid pipeline through a pipeline and connected in series with a valve, an electronic flowmeter and a transfer pump, and the pH adjusting discharge outlet 403 is connected to the concentration kettle 5 and the crystallization kettle 6 through a second three-way valve 10.

[0027] The top of the concentration kettle 5 is provided with a concentration liquid inlet 501 and a concentration gas outlet 502, the bottom is provided with a concentration liquid outlet 503, and the outer wall is provided with a concentration constant-temperature heat exchanger 504, the concentration gas outlet is connected to a recovered water storage tank through a pipeline and connected in series with a valve and a vacuum pump, and the concentration liquid outlet 503 is connected to the mother liquor liquid inlet 202 through a pipeline and connected in series with a valve, an electronic flowmeter and a transfer pump.

[0028] The top of the crystallization kettle 6 is provided with a crystallization feed inlet 601 and a crystallization water inlet 602, the bottom is provided with a crystallization discharge outlet 603 and a weighing module 604, and the outer wall is provided with a crystallization constant-temperature heat exchanger 605, the crystallization water inlet 602 is connected to a pure water pipeline through a pipeline and connected in series with a valve, an electronic flowmeter and a transfer pump, and the crystallization discharge outlet 603 is connected to the rotary furnace 7 and a crystallization water recovery pipeline through a third three-way valve 11.

[0029] The left end of the rotary furnace is provided with an inlet 701, and the right end is provided with an outlet 702, and the outlet 702 is connected to a product storage tank through a pipeline and connected in series with a valve.

[0030] In the device, the left end of the first three-way valve 9 is connected to the dissolution liquid outlet 102 through a pipeline and connected in series with a solenoid valve, an electronic flowmeter and an electromagnetic pump, the upper end is connected to the mother liquor liquid outlet 203 through a pipeline and connected in series with a solenoid valve, an electronic flowmeter and an electromagnetic pump, and the right end is connected to the reaction inlet 301 through a pipeline.

[0031] The left end of the second three-way valve 10 is connected to the crystallization feed inlet 601 through a pipeline and connected in series with a valve and a transfer pump, the upper end is connected to the pH adjusting discharge outlet 403 through a pipeline and connected in series with a valve, and the right end is connected to the concentration liquid inlet 501 through a pipeline and connected in series with a valve, an electronic flowmeter and a transfer pump.

[0032] The left end of the third three-way valve 11 is connected to the crystallization discharge outlet 603 through a pipeline and connected in series with a valve, the upper end is connected to the rotary furnace inlet 701 through a pipeline and connected in series with a valve and a transfer pump, and the right end is connected to the crystallization water recovery pipeline and connected in series with a valve and a transfer pump.

[0033] The PLC interlocking device 8 is connected with the electronic flowmeter at the left end of the first three-way valve and the electromagnetic valve and the electronic flowmeter in series at the upper end of the first three-way valve through data lines to form interlocking.

[0034] The dissolving kettle, the mother liquor kettle, the pH adjusting kettle, the concentration kettle and the crystallization kettle can be connected in parallel according to actual needs, and N≥2.

[0035] Specifically, the main raw material equipment specifications in the device are as follows: the dissolving kettle is a 5000L enamel kettle, and two are connected in parallel; the mother liquor kettle, the pH adjusting kettle, the concentration kettle and the crystallization kettle are all 3000L enamel kettles, and two are connected in parallel; the inner diameter of the tubular reactor is 8cm, and the length is 50m. The raw materials are all commercially available.

[0036] PLC parameter setting:

[0037] According to the content of sodium sarcosinate in the dissolving kettle and the mother liquor kettle and the content of cyanamide in the mother liquor kettle, the real-time flow rate of the electronic flowmeter at the left end of the first three-way valve and the multiple relationship of the real-time flow rate of the electronic flowmeter at the upper end of the first three-way valve are calculated according to the molar ratio of 1:1 of sodium sarcosinate and cyanamide. The real-time flow rate signal of the electronic flowmeter at the left end of the first three-way valve received by the PLC interlocking device sends the control signal of the electromagnetic valve and the electromagnetic pump at the upper end of the first three-way valve to realize the above multiple relationship, and real-time monitoring is performed through the electronic flowmeter at the upper end of the first three-way valve.

[0038] Production example of the device

[0039] Step 1: Pump the prepared sodium sarcosinate aqueous solution with pH value of 9.0 and mass fraction of 35% into the dissolving kettle 1 through the dissolving inlet 101, pump the cyanamide aqueous solution with mass fraction of 40% into the mother liquor kettle 2 through the mother liquor supplement inlet 201, control the temperature of the tubular reactor 3 at 60~90℃ through the reaction constant temperature heat exchanger 303, open the corresponding valve, and control the flow rate of sodium sarcosinate and cyanamide through the first three-way valve 9 and the reaction inlet 301 into the tubular reactor 3 according to a certain proportion through the PLC interlocking device 8 to react.

[0040] Step 2: After 1~2h, the reaction liquid flows out from the reaction outlet 302, is pumped into the pH adjusting kettle through the pH adjusting inlet 401, stirring is started, the temperature is lowered to 20℃ through the pH adjusting constant temperature heat exchanger 404, a certain mass of reaction liquid is enriched, hydrochloric acid is added dropwise through the pH adjusting inlet 402 to adjust the pH of the system to 7.5, stirring is stopped, solid-liquid separation is performed through the second three-way valve 10, the filtrate is pumped into the concentration kettle 5 through the pH adjusting outlet 403 and the concentration inlet 501 in sequence, and the remaining wet solid is introduced into the crystallization kettle 6 through the crystallization inlet 601.

[0041] The liquid in the concentration kettle 5 is heated by the concentration constant temperature heat exchanger 504 under the action of the vacuum pump, and after the outer steam part of water is evaporated, the filtered liquid is pumped into the parallel mother liquor kettle for standby use through the concentration outlet port (503) and the mother liquor inlet port (202) under the action of the filtration pump.

[0042] Step 3: according to the wet solid mass obtained by the crystallization weighing module 604, a certain amount of pure water is pumped in through the crystallization water inlet 602, the stirring is started, the temperature is raised to 80 DEG C through the crystallization constant temperature heat exchanger 605, after the solid in the crystallization kettle 6 is completely dissolved, the temperature is lowered to 10 DEG C at a certain rate, the solid-liquid separation is carried out through the third three-way valve 11, the solid is put into the rotary furnace 7 through the rotary inlet 701 for drying, after 30-60 min, the dried product is discharged from the rotary outlet 702, and the product is N-methyl guanidino acetic acid monohydrate with a purity of more than 99.9%.

[0043] The above is the preferred embodiment of the present application, and for those skilled in the art, according to the teaching of the present application, the changes, modifications, replacements and modifications of the embodiments without departing from the principles and spirits of the present application still fall within the protection scope of the present application.

Claims

1. An apparatus for producing N-methylguanidinoacetic acid, characterized in that, It includes a dissolving kettle (1), a mother liquor kettle, a tubular reactor, a pH adjusting kettle, a concentration kettle, a crystallization kettle and a rotary furnace, the outer wall of the dissolving kettle (1) is provided with a dissolving constant temperature heat exchanger (103), the bottom is provided with a dissolving outlet (102) which is connected with the reaction inlet (301) of the tubular reactor through a first three-way joint (9); The bottom of the mother liquor kettle is provided with a mother liquor outlet (203) which is connected with the first three-way joint, the outer wall is provided with a mother liquor constant temperature heat exchanger (204), and the top of the mother liquor kettle is provided with a mother liquor inlet (202) which is communicated with the concentration outlet (503) of the bottom of the concentration kettle; The outer wall of the tubular reactor is sleeved with a reaction constant temperature heat exchanger (303), and the reaction outlet (302) is communicated with the top pH adjusting feed inlet (401) of the pH adjusting kettle; The bottom of the crystallization kettle is provided with a crystallization outlet (603) which is connected with the rotary furnace and a crystallization water recovery pipeline.

2. The apparatus for producing N-methylguanidine acetic acid according to claim 1, characterized by, The dissolving inlet (101) of the dissolving kettle (1) is connected with a pipeline, and valves, an electronic flow meter and a transmission pump are connected in series on the pipeline, and the outlet (102) is connected with the first three-way joint (9).

3. The apparatus for producing N-methylguanidine acetic acid according to claim 2, characterized by, The mother liquor outlet (203) of the mother liquor kettle is connected with a mother liquor pipeline, and valves, an electronic flow meter and a transmission pump are arranged on the pipeline, and the electronic flow meter and the valves on the mother liquor pipeline are connected with the transmission pump on the dissolving pipeline to form a interlocking structure. The top of the mother liquor kettle is provided with a mother liquor supplement inlet (201), and valves, an electronic flow meter and a transmission pump are connected in series on the supplement pipeline connected with the mother liquor supplement inlet (201), and the mother liquor inlet (202) of the mother liquor kettle is connected with a pipeline, and valves, an electronic flow meter and a transmission pump are connected in series on the pipeline.

4. The apparatus for producing N-methylguanidine acetic acid according to claim 1, characterized by, The top of the pH adjusting kettle is provided with a pH adjusting feed inlet (401) and a pH adjusting inlet (402), and the bottom is provided with a pH adjusting outlet (403), and the outer wall is provided with a pH adjusting constant temperature heat exchanger (404), the pH adjusting feed inlet (401) is connected with the reaction outlet (302) through a pipeline, and valves, an electronic flow meter and a transmission pump are connected in series on the pipeline, the pH adjusting inlet (402) is connected with a hydrochloric acid pipeline through a pipeline, and valves, an electronic flow meter and a transmission pump are connected in series on the pipeline, and the pH adjusting outlet (403) is connected with the concentration kettle and the crystallization kettle through the second three-way joint (10).

5. The apparatus for producing N-methylguanidine acetic acid according to claim 1, characterized by, The top of the concentration kettle is provided with a concentration inlet (501) and a concentration gas outlet (502), the bottom is provided with a concentration outlet (503), the outer wall is provided with a concentration constant temperature heat exchanger (504), the concentration gas outlet is connected with a recovered water storage tank through a pipeline, and valves and a vacuum pump are connected in series on the pipeline, and the concentration outlet (503) is connected with the mother liquor inlet (202) through a pipeline, and valves, an electronic flow meter and a filtration pump are connected in series on the pipeline.

6. The apparatus for producing N-methylguanidine acetic acid according to claim 1, characterized by, The top of the crystallization kettle is provided with a crystallization feed port (601) and a crystallization water inlet (602), the bottom is provided with a crystallization discharge port (603) and a crystallization weighing module (604), the outer wall is provided with a crystallization constant-temperature heat exchanger (605), the crystallization water inlet (602) is connected with a pure water pipeline through a pipeline and is connected with a valve, an electronic flow meter and a transmission pump in series, and the crystallization discharge port (603) is connected with a rotary furnace and a crystallization water recovery pipeline through a third three-way valve (11).

7. The apparatus for producing N-methylguanidine acetic acid according to claim 1, characterized by, The left end of the rotary furnace is provided with a rotary furnace inlet (701), and the right end is provided with a rotary furnace outlet (702), and the rotary furnace outlet (702) is connected with a product storage tank through a pipeline and is connected with a valve in series.

8. The apparatus for producing N-methylguanidine acetic acid according to claim 1, characterized by, The dissolution kettle, the mother liquor kettle, the pH adjusting kettle, the concentration kettle and the crystallization kettle need N parallel connections, and N≥2.

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