CN115869880A - A kind of preparation method and device of D-serine - Google Patents

Abstract

The present invention relates to the field of organic chemistry, in particular to a preparation method and device for D-serine, including a stirrer, a scrubber, a dissociator, a suction filter and a drier. The stirrer includes a support assembly, a stirring assembly and a separation assembly, and The assembly includes a shell and a base. The stirring assembly includes a top cover, lifter, stirring motor, stirring rod and blades. The separation assembly includes an air pump, a liquid storage bottle, a filter, a support ring and a support rod. The support rod can rotate relative to the top cover. The filter screen separates the solid and the liquid, the air pump is connected to the liquid storage bottle, and the air pump is started to generate negative pressure in the liquid storage bottle to separate the D-serine preform that has reacted in the shell, the liquid enters the liquid storage bottle, and the solid remains On the filter net, start the lifter to lift the top cover, lift the support ring at the same time, and then turn the support rod to take out the solids, so that the solids and liquids can be separated directly after the stirring is completed to improve work efficiency.

Description

A kind of preparation method and device of D-serine

technical field

The invention relates to the field of organic chemistry, in particular to a method and device for preparing D-serine.

Background technique

As a non-protein optically active amino acid, D-serine has special physiological properties. It is widely used in pharmaceutical research, organic synthesis, peptide synthesis and other fields. Especially in the pharmaceutical industry, D-serine can be used as an auxiliary drug. Effectively improve the positive symptoms, negative symptoms and cognitive impairment of schizophrenic patients, so D-serine is widely used in the field of neurology, and it has broad application value in the development of new drugs.

The existing D-serine needs to be taken out completely after stirring in the preparation process for solid-liquid separation, which reduces the work efficiency.

Contents of the invention

The purpose of the present invention is to provide a preparation method and device for D-serine, aiming at directly performing solid-liquid separation after stirring to improve work efficiency.

In order to achieve the above object, in a first aspect, the present invention provides a D-serine preparation device, including a stirrer, a scrubber, a dissociator, a suction filter and a dryer, and the stirrer includes a support assembly, a stirring assembly and The separation assembly, the support assembly includes a shell and a base, the shell is fixedly connected to the base and is located on one side of the base, the stirring assembly includes a top cover, a lifter, a stirring motor, a stirring rod and blades, The top cover is slidably connected with the shell and is located on one side of the shell, the lifter is connected with the top cover, the stirring motor is arranged on the top cover, the stirring rod is connected with the The output end of the stirring motor is fixedly connected and located in the top cover, the blade is fixedly connected with the stirring rod and located in the top cover, and the separation assembly includes an air pump, a liquid storage bottle, a filter screen, a support a ring and a support rod, the support rod is rotatably connected to the top cover and located on a side of the top cover close to the housing, the support ring is fixedly connected to the support rod and located inside the housing, The filter screen is arranged at the bottom of the support ring, the liquid storage bottle is arranged at one side of the filter screen, and the air pump communicates with the liquid storage bottle.

Wherein, the lifter includes a lifting cylinder and a lifting rod, the lifting cylinder is arranged on one side of the housing, and the lifting rod is fixedly connected to the output end of the lifting cylinder and the top cover.

Wherein, the stirring assembly further includes a sealing ring, the sealing ring is fixedly connected with the top cover, and is located on a side of the top cover close to the shell.

Wherein, the stirring rod includes a rod body, a support spring and a sliding rod, the rod body is fixedly connected to the output end of the stirring motor, the sliding rod is slidably connected to the rod body, and the blades are fixed on the sliding rod , the supporting spring is arranged between the rod body and the sliding rod.

Wherein, the housing has a positioning plate, and the positioning plate is located on a side of the housing close to the top cover.

In the second aspect, the present invention provides a method for preparing D-serine, comprising: mixing L-serine and S-phenylethanesulfonic acid at a molar ratio of 1:0.3 to 1.5 and adding an aromatic aldehyde catalyst into the agitator , stirring at a temperature of 70°C to 90°C for 4 to 8 hours;

Open the control valve to filter the liquid into the liquid collection bottle, and the filter cake stays on the filter net;

Start the elevator to drive the top cover to move up, and turn the support rod to pour out the filter cake.

After the filter cake is washed, dissociated, suction filtered and dried, the D-serine product is obtained.

Wherein, the added mass of the aromatic aldehyde catalyst is 1.0% to 5.0% of L-serine;

A preparation method and device of D-serine according to the present invention, the agitator includes a support assembly, a stirring assembly and a separation assembly, the support assembly includes a shell and a base, the shell is fixedly connected to the base, and is located at the One side of the base, the shell is supported by the base, the stirring assembly includes a top cover, a lifter, a stirring motor, a stirring rod and blades, the top cover is slidably connected with the shell, and is located at the One side of the shell, the lifter is connected with the top cover, the lifter can lift the top cover or allow the top cover to move down and close the shell, the stirring motor is arranged on the On the top cover, the stirring rod is fixedly connected to the output end of the stirring motor, and is located in the top cover, and the blade is fixedly connected to the stirring rod, and is located in the top cover, and the stirring motor The stirring rod can be driven to rotate, so that the blade can be driven to rotate. The separation assembly includes an air pump, a liquid storage bottle, a filter screen, a support ring and a support rod. The support rod is rotatably connected with the top cover and is located at The top cover is close to the side of the casing, so that the support rod can rotate relative to the top cover, the support ring is fixedly connected with the support rod, and is located in the casing, and the filter is arranged on The bottom of the support ring can separate solids and liquids through the filter screen, the liquid storage bottle is arranged on one side of the filter screen, the air pump communicates with the liquid storage bottle, and the air pump can be activated to Negative pressure is generated in the liquid storage bottle so that the D-serine preform that has completed the reaction in the housing is separated, so that the liquid enters the liquid storage bottle, the solid remains on the filter, and then starts the The lifter lifts the top cover, lifts the support ring at the same time, and then rotates the support rod to take out the solid therein, so that the solid and liquid can be directly separated after the stirring is completed to improve work efficiency.

Description of drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. Those skilled in the art can also obtain other drawings based on these drawings without creative work.

Fig. 1 is a structural diagram of a D-serine preparation device of the present invention.

Fig. 2 is a structural diagram of the stirrer of the present invention.

Fig. 3 is a left structural view of the stirrer of the present invention.

Fig. 4 is a schematic cross-sectional view of the stirrer of the present invention.

Fig. 5 is a partially enlarged view of detail A in Fig. 4 .

Fig. 6 is a second cross-sectional schematic view of the stirrer of the present invention.

Fig. 7 is a flowchart of a preparation method of D-serine of the present invention.

1-Agitator, 2-Scrubber, 3-Separator, 4-Suction filter, 5-Dryer, 11-Support component, 12-Stir component, 13-Separation component, 111-Shell, 112-Base, 113 -connecting rod, 114-feeding plate, 121-top cover, 122-lifter, 123-stirring motor, 124-stirring rod, 125-blade, 126-sealing ring, 131-air pump, 132-liquid storage bottle, 133 -Filter screen, 134-support ring, 135-support rod, 136-driver, 1111-positioning plate, 1221-lift cylinder, 1222-lift rod, 1241-rod body, 1242-support spring, 1243-sliding rod, 1351-the first Second gear, 1361-first gear, 1362-driving motor, 1363-limit post.

Detailed ways

Embodiments of the present invention are described in detail below, examples of which are shown in the drawings, wherein the same or similar reference numerals designate the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the figures are exemplary and are intended to explain the present invention and should not be construed as limiting the present invention.

In describing the present invention, it should be understood that the terms "length", "width", "upper", "lower", "front", "rear", "left", "right", "vertical", The orientation or positional relationship indicated by "horizontal", "top", "bottom", "inner", "outer", etc. are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than Nothing indicating or implying that a referenced device or element must have a particular orientation, be constructed, and operate in a particular orientation should therefore not be construed as limiting the invention. In addition, in the description of the present invention, "plurality" means two or more, unless otherwise specifically defined.

Please refer to Figures 1 to 6. In the first aspect, the present invention provides a D-serine preparation device:

Comprising a mixer 1, a scrubber 2, a dissociator 3, a suction filter 4 and a dryer 5, the mixer 1 includes a support assembly 11, a stirring assembly 12 and a separation assembly 13, and the support assembly 11 includes a housing 111 and a base 112, the housing 111 is fixedly connected to the base 112, and is located on one side of the base 112, the stirring assembly 12 includes a top cover 121, a lifter 122, a stirring motor 123, a stirring rod 124 and a blade 125, the The top cover 121 and

, the housing 111 is slidingly connected and located on one side of the housing 111, the lifter 122 is connected to the top cover 121, the stirring motor 123 is arranged on the top cover 121, and the stirring rod 124 It is fixedly connected with the output end of the stirring motor 123, and is located in the top cover 121, and the blade 125 is fixedly connected with the stirring rod 124, and is located in the top cover 121, and the separation assembly 13 includes an air pump 131, a liquid storage bottle 132, a filter screen 133, a support ring 134 and a support rod 135, the support rod 135 is rotatably connected to the top cover 121, and is located on the side of the top cover 121 close to the housing 111, the The support ring 134 is fixedly connected with the support rod 135 and is located in the housing 111, the filter screen 133 is arranged at the bottom of the support ring 134, and the liquid storage bottle 132 is arranged at the bottom of the filter screen 133. On one side, the air pump 131 communicates with the liquid storage bottle 132 .

In this embodiment, the agitator 1 includes a support assembly 11, a stirring assembly 12 and a separation assembly 13, the support assembly 11 includes a housing 111 and a base 112, the housing 111 is fixedly connected to the base 112, and is located at One side of the base 112 is used to support the housing 111 through the base 112. The stirring assembly 12 includes a top cover 121, a lifter 122, a stirring motor 123, a stirring rod 124 and a blade 125. The top cover 121 is slidably connected with the casing 111 and is located on one side of the casing 111. The lifter 122 is connected with the top cover 121, and the top cover 121 can be lifted or the top cover 121 can be lifted by the lifter 122. The cover 121 moves down and the housing 111 is closed, the stirring motor 123 is arranged on the top cover 121, the stirring rod 124 is fixedly connected with the output end of the stirring motor 123, and is located in the top cover 121 , the blade 125 is fixedly connected with the stirring rod 124, and is located in the top cover 121, the stirring motor 123 can drive the stirring rod 124 to rotate, thereby driving the blade 125 to rotate, the separation assembly 13 includes an air pump 131, a liquid storage bottle 132, a filter screen 133, a support ring 134 and a support rod 135, the support rod 135 is rotatably connected to the top cover 121, and is located at one side of the top cover 121 close to the housing 111 side, so that the support rod 135 can rotate relative to the top cover 121, the support ring 134 is fixedly connected with the support rod 135, and is located in the housing 111, and the filter screen 133 is arranged on the support ring 134, solids and liquids can be separated through the filter screen 133, the liquid storage bottle 132 is arranged on one side of the filter screen 133, the air pump 131 communicates with the liquid storage bottle 132, and starts the The air pump 131 can generate negative pressure in the liquid storage bottle 132 so that the D-serine preform that has been reacted in the shell 111 is separated, so that the liquid enters the liquid storage bottle 132, and the solid remains in the liquid storage bottle 132. on the filter screen 133, then start the lifter 122 to lift the top cover 121, lift the support ring 134 simultaneously, and then turn the support rod 135 to take out the solid therein, so that the solid can be directly treated after the stirring is completed. Separated from the liquid to improve work efficiency.

Further, the lifter 122 includes a lifting cylinder 1221 and a lifting rod 1222, the lifting cylinder 1221 is arranged on one side of the housing 111, the lifting rod 1222 is connected to the output end of the lifting cylinder 1221 and the top The cover 121 is fixedly connected.

In this embodiment, the lifting cylinder 1221 can drive the lifting rod 1222 to move up and down, thereby driving the top cover 121 to move up and down.

Further, the stirring assembly 12 also includes a sealing ring 126 , which is fixedly connected to the top cover 121 and located on a side of the top cover 121 close to the casing 111 .

In this embodiment, the gap between the top cover 121 and the housing 111 can be sealed by the sealing ring 126 to avoid liquid leakage.

Further, the stirring rod 124 includes a rod body 1241, a support spring 1242 and a sliding rod 1243, the rod body 1241 is fixedly connected to the output end of the stirring motor 123, and the sliding rod 1243 is slidingly connected to the rod body 1241, so The blade 125 is fixed on the sliding rod 1243 , and the support spring 1242 is arranged between the rod body 1241 and the sliding rod 1243 .

In this embodiment, the sliding rod 1243 can slide on the rod body 1241, so that when the blade 125 rotates, the sliding rod 1243 can be driven down by the reaction force of the blade 125 to pull the The supporting spring 1242 makes it possible to move the blade 125 up and down, so that the stirring is more sufficient.

Further, the housing 111 has a positioning plate 1111, and the positioning plate 1111 is located on the side of the housing 111 close to the top cover 121; the support assembly 11 also includes a connecting rod 113 and a material taking plate 114, the The connecting rod 113 is arranged in the positioning plate 1111 , and the picking plate 114 is rotatably connected with the connecting rod 113 and located on one side of the housing 111 .

In this embodiment, the positioning plate 1111 can facilitate the placement of the material taking plate 114 , and slide relative to the positioning plate 1111 between the top cover 121 and the casing 111 to take out solid materials. Wherein the connecting rod 113 can slide relative to the positioning plate 1111, and the pick-up plate 114 can follow the connecting rod 113 and enter between the top cover 121 and the outer shell 111, making it more convenient to use.

Further, the separation assembly 13 also includes a driver 136, and the driver 136 is arranged on one side of the support rod 135; The rod 135 has a second gear 1351, the drive motor 1362 is arranged on one side of the housing 111, the first gear 1361 is fixedly connected to the output end of the drive motor 1362, and is close to the second gear 1351, The limiting column 1363 is disposed on one side of the second gear 1351 .

In this embodiment, the driver 136 can drive the support rod 135 to rotate, thereby automatically driving the support ring 134 to turn over, specifically, when the top cover 121 is lifted, the first gear 1361 Meshing with the second gear 1351, the driving motor 1362 can drive the support rod 135 to rotate, and the limit column 1363 can limit the rotation position of the second gear 1351, making it more convenient to use.

In the second aspect, please refer to Figure 7, the present invention also provides a method for preparing D-serine, including:

S101 Mix L-serine and S-phenylethanesulfonic acid according to the molar ratio of 1:0.3~1.5 and add aromatic aldehyde catalyst into the mixer 1, stir at 70℃~90℃ for 4~8 hours ;

S102 Open the control valve to suction filter the liquid into the liquid collection bottle, leaving the filter cake on the filter screen 133;

S103 Start the lifter 122 to drive the top cover 121 to move up, and turn the support rod 135 to pour out the filter cake.

S104 Washing, dissociating, suction filtering and drying the filter cake to obtain the D-serine product.

Further, the added mass of the aromatic aldehyde catalyst is 1.0% to 5.0% of L-serine;

This method saves the racemization step, avoids entrainment and precipitation phenomenon that may be caused by the increase of enantiomer concentration, thereby reducing the loss of enantiomer, effectively improving the resolution efficiency and the optical purity of the target product D-serine, and at the same time, The chiral resolving agent S-phenylethanesulfonic acid recovered from the filtrate of the filter cake, as well as the organic solvent and aromatic aldehyde catalyst in the mother liquor can all be recycled, thereby greatly reducing the process cost and being suitable for industrial production.

What is disclosed above is only a preferred embodiment of the present invention, and of course it cannot limit the scope of rights of the present invention. Those of ordinary skill in the art can understand all or part of the process for realizing the above embodiments, and according to the rights of the present invention The equivalent changes required still belong to the scope covered by the invention.

Claims (7)

1. A preparation device for D-serine, characterized in that, It includes an agitator, a scrubber, a separator, a suction filter and a dryer, the agitator includes a support assembly, a stirring assembly and a separation assembly, the support assembly includes a shell and a base, the shell is fixedly connected to the base, And located on one side of the base, the stirring assembly includes a top cover, a lifter, a stirring motor, a stirring rod and blades, the top cover is slidably connected with the housing, and is located on one side of the housing, the The lifter is connected with the top cover, the stirring motor is arranged on the top cover, the stirring rod is fixedly connected with the output end of the stirring motor, and is located in the top cover, and the blades are connected with the The stirring rod is fixedly connected and located in the top cover. The separation assembly includes an air pump, a liquid storage bottle, a filter screen, a support ring and a support rod. The support rod is rotatably connected with the top cover and is located in the top cover. The cover is close to one side of the housing, the support ring is fixedly connected with the support rod and located inside the housing, the filter is arranged at the bottom of the support ring, and the liquid storage bottle is arranged at the bottom of the support ring. On one side of the filter screen, the air pump communicates with the liquid storage bottle. 2. the preparation device of a kind of D-serine as claimed in claim 1, is characterized in that, The lifter includes a lifting cylinder and a lifting rod, the lifting cylinder is arranged on one side of the housing, and the lifting rod is fixedly connected with the output end of the lifting cylinder and the top cover. 3. the preparation device of a kind of D-serine as claimed in claim 2, is characterized in that, The stirring assembly further includes a sealing ring, which is fixedly connected to the top cover and located on a side of the top cover close to the shell. 4. the preparation device of a kind of D-serine as claimed in claim 3, is characterized in that, The stirring rod includes a rod body, a supporting spring and a sliding rod, the rod body is fixedly connected to the output end of the stirring motor, the sliding rod is slidably connected to the rod body, and the blades are fixed on the sliding rod, so The supporting spring is arranged between the rod body and the sliding rod. 5. the preparation device of a kind of D-serine as claimed in claim 4, is characterized in that, The housing has a positioning plate, and the positioning plate is located on a side of the housing close to the top cover. 6. A preparation method of D-serine, applied to the preparation device of D-serine according to any one of claims 1-5, characterized in that, Including: mixing L-serine and S-phenylethanesulfonic acid according to the molar ratio of 1:0.3~1.5, adding aromatic aldehyde catalysts into the stirrer, and stirring at a temperature of 70°C~90°C for 4~8 hours ; Open the control valve to filter the liquid into the liquid collection bottle, and the filter cake stays on the filter net; Start the lifter to move the top cover up, and turn the support rod to pour out the filter cake; After the filter cake is washed, dissociated, suction filtered and dried, the D-serine product is obtained. 7. the preparation method and the device of a kind of D-serine as claimed in claim 6, it is characterized in that, The added mass of the aromatic aldehyde catalyst is 1.0%-5.0% of the L-serine.

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