CN105330078A - Method for recovering catalyst in B4 workshop section in pyridinium salt production - Google Patents

Abstract

The invention relates to a method for recovering a catalyst in a B4 workshop section in pyridinium salt production. The method comprises the following steps: 1, putting 1m<3> of catalyst-containing wastewater generated in the B4 workshop section in a single effect evaporator, and carrying out reduced pressure concentration to obtain 200L of a concentrate liquid; 2, cooling the concentrate liquid in a layering kettle to 10DEG C, adding 1m<3> of dichloromethane to form extraction phase and a water phase layering, and separating the dichloromethane-containing extraction phase to leave the water layer; 3, adding the water layer left after layering to 0.1L of ammonia water while stirring, ammonifying, and adding hydrochloric acid to adjust the pH value to 2.5-3.0; and 4, carrying out press filtration on the adjusted water layer through a filter press to obtain a workable catalyst. Concentration and extraction are successively carried out to recover the catalyst and recycle parts of materials, so the cost is saved, the yield is improved, and distilled water can return to a production line and is used, thereby multiple purposes are achieved.

Description

The catalyst recovery method of B4 workshop section in pyridinium salt production

Technical field:

The present invention relates to a kind of method of bulk drug pyridine hydrochloride catalyst recovery mode.

Background technology:

Pyridine hydrochloride is the bulk drug producing stomach medicine omeprazole, full name 2-chloromethyl, 3,4-dimethoxy pyridine hydrochloride.The production of pyridine hydrochloride, existing manufacturer both domestic and external mainly adopts methyl maltol through esterification, ammonification, chlorination, oxidation, alcoholization, anhydridization and salify refinement, production process is methyl maltol logical ammoniacal liquor ammonification after dimethyl sulfate esterification, add phosphorus oxychloride chlorination again, drip hydrogen peroxide oxidation again, add methyl alcohol alcoholization, add aceticanhydride anhydridization, after adding sulfur oxychloride salify, add the finished product that dehydrated alcohol is refined.But containing a large amount of catalyzer sodium wolframates in the waste water that B4 oxidation section produces, along with waste water is processed, one is increased the weight of environmental pollution, but increases production cost.

Summary of the invention

Object of the present invention is exactly to solve the shortcoming existed in prior art, the catalyst recovery method of B4 workshop section in a kind of pyridinium salt production provided.

The technical solution used in the present invention is as follows;

The catalyst recovery method of B4 workshop section in pyridinium salt production, is characterized in that comprising the following steps:

What a. B4 workshop section produced puts into single-effect evaporator containing containing wastewater from catalyst 1 cube, carries out concentrating under reduced pressure and obtains 200L concentrated solution;

B. the 200L concentrated solution after concentrated is put into layering still, after cooling to 10 degree, adds the organic impurity in 1 cube of dichloromethane extraction concentrated solution, and form extraction phase and aqueous phase layering, after the extraction phase containing methylene dichloride is isolated, leave water layer;

C. water layer layering stayed, after adding the ammonification of 0.1L ammoniacal liquor, then adds hydrochloric acid PH is adjusted to 2.53.0 under whipped state;

D. the water layer will regulated, after pressure filter press filtration, can obtain spendable catalyzer.

The waste water layer containing catalyzer after the present invention mainly uses the 4th stage oxidation workshop section (i.e. B4 workshop section) in pyridinium salt Production Flow Chart, first methylene dichloride layering is put into after putting into the cooling of layering still after carrying out concentrating under reduced pressure with single-effect evaporator, a part of organic impurity and recoverable material are removed, then ammoniacal liquor is added by after ammonification, adding hydrochloric acid regulates PH to carry out press filtration after 2 ~ 3, can use catalyzer.

The invention has the advantages that:

Catalyzer residual in catalyzer use procedure metal acid of attaching most importance to remains in the middle of waste water, if do not reclaimed, considerably increase the intractability of waste water, the present invention adopts and first concentrates the mode extracted afterwards, not only catalyst recovery is returned, and a part of material has been carried out reclaiming using, save cost, improve yield, the water simultaneously distilled, can get back to production line to use, be achieve many things at one stroke.

Embodiment:

(applying mechanically according to every still containing 1 cube, containing wastewater from catalyst layer a. by the normal temperature of i.e. B4 workshop section generation, main containing sodium wolframate in water) put into single-effect evaporator (1), carry out concentrating under reduced pressure (temperature 60 degree, reduced vacuum degree-0.09MPA, time about 1.5 hours, judges distillation end point according to evaporation), when the water yield that observation is evaporated away is about 0.6 side, check that residual concentrated solution liquid level is at 200L, just can put into layering still (2).

B. after the concentrated solution 200L of temperature 60 degree being put into layering still (2), open cold water for cooling is to about 10 degree, add 1 cube of methylene dichloride to extract, extraction temperature 10 degree, the time stirs 0.5 hour, leave standstill 1 hour, atmospheric pressure state, extraction agent (methylene dichloride) has extracted organic impurity and has formed extraction phase, and remaining water layer is exactly containing sodium tungstate solution, after by containing methylene dichloride slightly go want to separate, to stay time and use.

C. temperature layering stayed 10 degree containing the water layer 200L of sodium tungstate solution, after adding the ammonification of about 0.1L ammoniacal liquor under whipped state, then add hydrochloric acid PH be adjusted to 2.53.0, period attentional manipulation temperature do not surpass 10 degree.

D). by the water layer regulated, after pressure filter (5) press filtration, spendable catalyst liquid about 300L can be obtained.

Claims (1)

1. pyridinium salt produce in the catalyst recovery method of B4 workshop section, it is characterized in that comprising the following steps:

What a. B4 workshop section produced puts into single-effect evaporator containing containing wastewater from catalyst 1 cube, carries out concentrating under reduced pressure and obtains 200L concentrated solution;

B. the 200L concentrated solution after concentrated is put into layering still, after cooling to 10 degree, adds the organic impurity in 1 cube of dichloromethane extraction concentrated solution, and form extraction phase and aqueous phase layering, after the extraction phase containing methylene dichloride is isolated, leave water layer;

C. water layer layering stayed, after adding the ammonification of 0.1L ammoniacal liquor, then adds hydrochloric acid PH is adjusted to 2.5 3.0 under whipped state;

D. the water layer will regulated, after pressure filter press filtration, can obtain spendable catalyzer.