CN218076422U

CN218076422U - Famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device

Info

Publication number: CN218076422U
Application number: CN202222335985.6U
Authority: CN
Inventors: 张利
Original assignee: Wudi Rongchuan Chemical Technology Co ltd
Current assignee: Wudi Rongchuan Chemical Technology Co ltd
Priority date: 2022-09-02
Filing date: 2022-09-02
Publication date: 2022-12-20
Anticipated expiration: 2032-09-02

Abstract

The utility model discloses a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesizer. The synthesis device comprises a ketonization kettle arranged at the front end; an epichlorohydrin head tank and a sulfuric acid head tank are connected in parallel on the ketone reactor through pipelines; the ketonization kettle is also connected with a water head tank through a pipeline; the rear end of the ketonizing kettle is connected with a centrifugal machine through a pipeline; the rear end of the centrifuge is connected with a mother liquor ground trough through a pipeline; the synthesis device also comprises a refining distillation kettle. The 1.3-dichloropropanol is prepared by using the device to open the ring of the epichlorohydrin in acid, so that the cost of raw materials is greatly reduced, the reaction temperature can be increased, the temperature is increased to about 30 ℃ to 45-50 ℃, and the time of ketonic equilibrium reaction is shortened to 2 hours from the original 4 hours.

Description

Famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device

Technical Field

The utility model belongs to the field of drug intermediate production equipment, in particular to a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesizer.

Background

1.3-dichloroacetone is one of the key starting materials of famotidine double salt products, potassium dichromate or sodium dichromate is mostly used as an oxidant in the current domestic production process, chromium oxide is also used as an oxidant in literature reports, but the serious harm of chromium ions to water quality and human bodies cannot be eliminated, although the chromium salt oxidation process is abolished through process optimization, a large amount of concentrated sulfuric acid is used to influence wastewater treatment and environment, the problem of easy decomposition of high-concentration hydrogen peroxide is also caused to bring difficulties to storage and transportation, and the instability directly influences the quality of the 1.3-dichloroacetone product, so that the quality problem of the 1.3-dichloroacetone needs to be solved, and the problem of stable quality of the nizatidine product caused by the quality problem is mainly solved.

At present, 1, 3-dichloroacetone is produced by ketonizing 1, 3-dichloropropanol, and the specific reaction is as follows:

SUMMERY OF THE UTILITY MODEL

The utility model provides a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesizer, which can reduce the production cost and improve the reaction speed.

In order to achieve the above object, the utility model provides a following technical scheme: a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device comprises a ketonizing kettle arranged at the front end; an epichlorohydrin head tank and a sulfuric acid head tank are connected in parallel on the ketone reactor through pipelines; the ketonizing kettle is also connected with a water head tank through a pipeline; the rear end of the ketonizing kettle is connected with a centrifugal machine through a pipeline; the rear end of the centrifuge is connected with a mother liquor ground trough through a pipeline; the synthesis device also comprises a refining distillation kettle.

Preferably, the refining distillation kettle is connected with a first condenser through a pipeline; the rear end of the first condenser is connected with a waste liquid receiving tank through a pipeline.

Preferably, a pump is installed at the rear end of the mother liquid ground tank; the rear end of the pump is connected with a wastewater concentration kettle through a pipeline; the rear end of the wastewater concentration kettle is connected to a waste liquid receiving tank through a pipeline; and the wastewater concentration kettle is connected with a second condenser through a pipeline.

Preferably, ketone cauldron, epichlorohydrin elevated tank and sulphuric acid elevated tank set up two sets ofly, and water elevated tank sets up one set ofly, by two ketone cauldron sharing.

Compared with the prior art, the beneficial effects of the utility model are that: the 1.3-dichloropropanol is prepared by ring opening of the epichlorohydrin in acid, so that the cost of raw materials is greatly reduced, the reaction temperature can be increased, the temperature is increased to about 30 ℃ to 45-50 ℃, and the time of the ketonization equilibrium reaction is shortened to 2 hours from the original 4 hours.

Other features of the present disclosure and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.

Drawings

In order to more clearly illustrate the embodiments of the present disclosure or technical solutions in related arts, the drawings used in the description of the embodiments or related arts will be briefly introduced below, it is obvious that the drawings in the following description are only embodiments of the present disclosure, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.

FIG. 1 is an overall view of the synthesizing device of the present invention;

in the figure: 1. ketone cauldron, 2, epichlorohydrin elevated tank, 3, sulphuric acid elevated tank, 4, water elevated tank, 5, centrifuge, 6, mother liquor geosyncline, 7, refined distillation cauldron, 8, first condenser, 9, waste liquid receiving tank, 10, pump, 11, waste water concentration cauldron, 12, second condenser.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.

Unless specifically stated otherwise, the relative arrangement of parts and steps, numerical expressions, and numerical values set forth in these embodiments do not limit the scope of the present invention. Meanwhile, it should be understood that the sizes of the respective portions shown in the drawings are not drawn in an actual proportional relationship for the convenience of description. Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, further discussion thereof is not required in subsequent figures.

For ease of description, spatially relative terms such as "over 8230 \ 8230;,"' over 8230;, \8230; upper surface "," above ", etc. may be used herein to describe the spatial relationship of one device or feature to another device or feature as shown in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if a device in the figures is turned over, devices described as "above" or "on" other devices or configurations would then be oriented "below" or "under" the other devices or configurations. Thus, the exemplary terms "at 8230; \8230; above" may include both orientations "at 8230; \8230; above" and "at 8230; \8230; below". The device may be otherwise variously oriented (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.

Referring to fig. 1, the present invention provides a technical solution: a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device comprises a ketonization kettle 1 arranged at the front end; an epichlorohydrin head tank 2 and a sulfuric acid head tank 3 are connected in parallel on the ketone reactor 1 through pipelines; the ketonization kettle 1 is also connected with a water head tank 4 through a pipeline; the rear end of the ketonizing kettle 1 is connected with a centrifugal machine 5 through a pipeline; the rear end of the centrifuge 5 is connected with a mother liquor ground tank 6 through a pipeline; the synthesis apparatus further comprises a refining still 7.

The refining distillation kettle 7 is connected with a first condenser 8 through a pipeline; the rear end of the first condenser 8 is connected with a waste liquid receiving tank 9 through a pipeline. The rear end of the mother liquid ground tank 6 is provided with a pump 10; the rear end of the pump 10 is connected with a wastewater concentration kettle 11 through a pipeline; the rear end of the waste water concentration kettle 11 is connected to the waste liquid receiving tank 9 through a pipeline; the wastewater concentration kettle 11 is connected with a second condenser 12 through a pipeline. Ketonizing cauldron 1, epichlorohydrin elevated tank 2 and sulphuric acid elevated tank 3 set up two sets ofly, and water elevated tank 4 sets up and sets up a set ofly, by two ketonizing cauldron 1 sharing.

During the reaction, quantitative hydrochloric acid is pumped into the ketonizing kettle 1, a jacket of the reaction kettle is opened to freeze an inlet valve and an outlet valve, the temperature is controlled to be 20-25 ℃, the dropwise adding valve of the ring-opening epichlorohydrin elevated tank 2 is finished, and epichlorohydrin is dropwise added; after the reaction is finished at about 20 to 25 ℃ for 3 hours, pumping process water into the reaction kettle from a water head tank 4.

Adding potassium dichromate into the ketone kettle 1, stirring, dropwise adding sulfuric acid from a sulfuric acid head tank 3, controlling the dropwise adding temperature below 25 ℃, controlling the temperature to be 20-25 ℃ after the dropwise adding is finished, reacting for 4 hours, cooling to 0-5 ℃ after the dropwise adding is finished, and performing solid-liquid separation by a centrifuge 5 to obtain a 1.3-dichloroacetone crude product.

Adding the 1.3-dichloroacetone crude product into a refining distillation kettle 7, stirring, vacuum (less than or equal to-0.08 MPa), slowly heating, vacuum distilling, closing a heating valve when the temperature reaches 100-120 deg.C (no obvious liquid drop is dripped on a visual cup), and discharging the material when the temperature is hot to obtain the 1.3-dichloroacetone finished product.

Wherein the waste liquid generated by the centrifuge 5 is pumped into a waste water concentration kettle 11 and condensed into a waste liquid receiving tank 9, and the condensate liquid generated during distillation in the refining distillation kettle 7 flows into the waste liquid receiving tank 9 after passing through a first condenser 8. The waste liquid collected by the waste liquid receiving tank 9 is sent to a qualified environmental protection department for treatment.

Example 1:

a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device comprises a ketonization kettle 1 arranged at the front end; an epichlorohydrin head tank 2 and a sulfuric acid head tank 3 are connected in parallel on the ketone reactor 1 through pipelines; the ketonizing kettle 1 is also connected with a water head tank 4 through a pipeline; the rear end of the ketonizing kettle 1 is connected with a centrifuge 5 through a pipeline; the rear end of the centrifuge 5 is connected with a mother liquor ground tank 6 through a pipeline; the synthesis apparatus further comprises a refining still 7.

Example 2:

a famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device comprises a ketonization kettle 1 arranged at the front end; an epichlorohydrin head tank 2 and a sulfuric acid head tank 3 are connected in parallel on the ketone reactor 1 through pipelines; the ketonizing kettle 1 is also connected with a water head tank 4 through a pipeline; the rear end of the ketonizing kettle 1 is connected with a centrifuge 5 through a pipeline; the rear end of the centrifuge 5 is connected with a mother liquor ground tank 6 through a pipeline; the synthesis apparatus further comprises a refining still 7. The refining distillation kettle 7 is connected with a first condenser 8 through a pipeline; the rear end of the first condenser 8 is connected with a waste liquid receiving tank 9 through a pipeline. The rear end of the mother liquid ground tank 6 is provided with a pump 10; the rear end of the pump 10 is connected with a wastewater concentration kettle 11 through a pipeline; the rear end of the waste water concentration kettle 11 is connected to the waste liquid receiving tank 9 through a pipeline; the wastewater concentration kettle 11 is connected with a second condenser 12 through a pipeline. Ketonizing cauldron 1, epichlorohydrin elevated tank 2 and sulphuric acid elevated tank 3 set up two sets ofly, and water elevated tank 4 sets up and sets up a set ofly, by two ketonizing cauldron 1 sharing.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. A famotidine double-salt key intermediate 1, 3-dichloroacetone synthesis device is characterized in that: the synthesis device comprises a ketonizing kettle (1) arranged at the front end; an epichlorohydrin head tank (2) and a sulfuric acid head tank (3) are connected in parallel on the ketonizing kettle (1) through pipelines; the ketonizing kettle (1) is also connected with a water head tank (4) through a pipeline; the rear end of the ketonizing kettle (1) is connected with a centrifuge (5) through a pipeline; the rear end of the centrifuge (5) is connected with a mother liquor trough (6) through a pipeline; the synthesis device also comprises a refining distillation kettle (7).

2. The device for synthesizing the famotidine double-salt key intermediate 1, 3-dichloroacetone according to claim 1, which is characterized in that: the refining distillation kettle (7) is connected with a first condenser (8) through a pipeline; the rear end of the first condenser (8) is connected with a waste liquid receiving groove (9) through a pipeline.

3. The device for synthesizing the famotidine double-salt key intermediate 1, 3-dichloroacetone according to claim 1, which is characterized in that: a pump (10) is arranged at the rear end of the mother liquid ground tank (6); the rear end of the pump (10) is connected with a wastewater concentration kettle (11) through a pipeline; the rear end of the waste water concentration kettle (11) is connected to the waste liquid receiving tank (9) through a pipeline; and the wastewater concentration kettle (11) is connected with a second condenser (12) through a pipeline.

4. The device for synthesizing the famotidine double-salt key intermediate 1, 3-dichloroacetone according to claim 1, which is characterized in that: ketone cauldron (1), epichlorohydrin elevated tank (2) and sulphuric acid elevated tank (3) set up two sets ofly, and water elevated tank (4) set up and set up a set ofly, by two ketone cauldron (1) sharing.