CN105503701B - A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content - Google Patents
A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content Download PDFInfo
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- CN105503701B CN105503701B CN201410485039.7A CN201410485039A CN105503701B CN 105503701 B CN105503701 B CN 105503701B CN 201410485039 A CN201410485039 A CN 201410485039A CN 105503701 B CN105503701 B CN 105503701B
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- diphenoxylate hydrochloride
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Abstract
The invention discloses a kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, including dissolution extraction workshop section, at salt workshop section, refined packing department and mother liquid disposal recycle section.Pass through above-mentioned recovery processing technique, so that diphenoxylate hydrochloride is processed into the certified products that content reaches 98% or more by content less than 98% defective work, as meeting as defined in National Pharmacopeia qualified drug, defective work to handle former stock, it is sold in time after processing is qualified, the waste in production is avoided, economic benefit is improved.
Description
Technical field
The present invention relates to a kind of recovery processing techniques of the unqualified diphenoxylate hydrochloride of content.
Background technology
Diphenoxylate hydrochloride is a kind of performance chemical material medicine for acute and chronic functional diarrhea and chronic enteritis.
Diphenoxylate hydrochloride is 1- (3,3- diphenyl -3- cyanopropyls) -4- phenyl -4- piperidine ethyl formate hydrochloric acid
Salt.It is calculated by dry product, must not contain and be less than 98.0%.Chemical raw material drug in this product is closed by multi-step chemical synthesis unit
At, but in the production of synthetic hydrochloric acid diphenoxylate chemical raw material drug, it is low often inevitably to there are individual batch contents
In National Pharmacopeia required standard.And traditional methods such as decolourize, refine is used not improve defective work at all
C30H32N2O2HCl amounts, therefore always will appear the underproof product of content in producing, cause certain waste.
Invention content
For problem of the prior art, the present invention provides a kind of recovery processing works of the unqualified diphenoxylate hydrochloride of content
Content is processed into content less than the defective work of the diphenoxylate hydrochloride content of National Pharmacopeia required standard and reaches national medicine by skill
The diphenoxylate hydrochloride of allusion quotation required standard is effectively reduced waste.
In order to achieve the above object, the technical scheme is that：
A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, includes the following steps：
1）, dissolution extraction workshop section：Unqualified diphenoxylate hydrochloride and pure water are pressed 1：4 mixing, at 23~25 DEG C fully
A concentration of 10% sodium hydroxide solution is added in stirring and dissolving, and the pH value for reconciling solution is 8.5~9.0, is filtered after stirring evenly, and is removed
Mechanical admixture；Filtrate is pumped into extraction kettle, 15~25min is stirred, stands 20~30min, water phase is released and sets in container, toluene
Mutually separately deposit；Into the water phase of releasing be added toluene after be pumped into extraction kettle in, toluene amount be unqualified diphenoxylate hydrochloride amount 2~
2.5 times, stirring is stood, layering, separation, will be detached toluene obtained twice and mutually be merged；Pure water is added in combined toluene phase
Washing, the amount of pure water are 4~4.5 times of unqualified diphenoxylate hydrochloride amount, and stirring is stood, layering, separation；Toluene phase and water
Mutually place respectively；
2）, at salt workshop section：Step 1）Obtained toluene, which is mutually placed in, to be crystallized into salt oven, and 2mol/L hydrochloric acid is added and stirs into
Salt, -7 DEG C~-10 DEG C 1~1.5h of placement, centrifuge rejection filter after dryings, crystal salt are dried at 50 DEG C~80 DEG C and is made slightly
Product, filtrate are spare；
3）, filtrate handle recycle section：By step 2）Caustic lye of soda is added in the filtrate that middle centrifugation filters out and adjusts its PH
It is 7, toluene phase is layered immediately with water phase, and separation mutually concentrates toluene, and concentrate is added 2mol/L hydrochloric acid and is crystallized at salt, rejection filter
Drying is crude product；
4）, refined packing department：By step 2）With step 3）Crude product after middle drying crushes, it is added to a concentration of 25%~
In 30% ethanol solution, dissolving, washing, drying, then use pure water, drying, cross 20 mesh screens granulation, be dried in vacuo, powder
Broken, chemical examination, packaging.
Further, step 2）The interlayer for crystallizing into salt oven leads to chilled brine cooling.
Further, step 4）Described in vacuum drying temperature be：80~90 DEG C, negative pressure is 0.07~0.1MPA, time
It is 3~4 hours.
The beneficial effects of the invention are as follows：Pass through above-mentioned recovery processing technique so that diphenoxylate hydrochloride is less than by content
98% defective work is processed into the certified products that content reaches 98% or more, becomes and meets qualified drug as defined in National Pharmacopeia, from
And the defective work that can not handle former stock, it is sold in time after processing is qualified, avoids the waste in production, improved
Economic benefit.
Specific implementation mode
With reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, includes the following steps：
1）, dissolution extraction workshop section：Unqualified diphenoxylate hydrochloride and pure water are pressed 1：4 mixing, are sufficiently stirred at 25 DEG C
A concentration of 10% sodium hydroxide solution is added in dissolving, and the pH value for reconciling solution is 9, is filtered after stirring evenly, and mechanical admixture is removed；It will
Filtrate is pumped into extraction kettle, stirs 25min, stands 30min, releases water phase and sets in container, toluene is mutually separately deposited；To the water phase of releasing
It being pumped into extraction kettle after middle addition toluene, toluene amount is 2 times of unqualified diphenoxylate hydrochloride amount, and stirring is stood, layering, point
From will detach toluene obtained twice and mutually merge；Pure water is added in combined toluene phase, the amount of pure water is unqualified salt
4 times of sour diphenoxylate amount, stirring are stood, layering, separation；Toluene phase and water phase are placed respectively；
2）, at salt workshop section：Step 1）Obtained toluene, which is mutually placed in, to be crystallized into salt oven, and 2mol/L hydrochloric acid is added and stirs into
Salt, the interlayer for crystallizing into salt oven lead to chilled brine cooling, place 1.5h at -7 DEG C, centrifuge rejection filter after drying, is dried at 80 DEG C
It is dry.
3）, filtrate handle recycle section：By step 2）Caustic lye of soda is added in the filtrate that middle centrifugation filters out and adjusts its PH
It is 7, toluene phase is layered immediately with water phase, and separation mutually concentrates toluene, and concentrate is added 2mol/L hydrochloric acid and is crystallized at salt, rejection filter
Drying is crude product；
4）, refined packing department：Crude product after drying is crushed, is added in a concentration of 30% ethanol solution, dissolving,
Washing, drying, then pure water is used, the granulation of 20 mesh screens is crossed in drying, is 90 DEG C in temperature, negative pressure is 0.07~0.1MPA
It is 4 hours dry in vacuum environment, it crushes, chemical examination, pack.
Embodiment 2
A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, includes the following steps：
1）, dissolution extraction workshop section：Unqualified diphenoxylate hydrochloride and pure water are pressed 1：4 mixing, are sufficiently stirred at 23 DEG C
A concentration of 10% sodium hydroxide solution is added in dissolving, and the pH value for reconciling solution is 9, is filtered after stirring evenly, and mechanical admixture is removed；It will
Filtrate is pumped into extraction kettle, stirs 20min, stands 25min, releases water phase and sets in container, toluene is mutually separately deposited；To the water phase of releasing
It being pumped into extraction kettle after middle addition toluene, toluene amount is 2.5 times of unqualified diphenoxylate hydrochloride amount, and stirring is stood, layering,
Separation will detach toluene obtained and mutually merge twice；Pure water is added in combined toluene phase, the amount of pure water is unqualified
4.5 times of diphenoxylate hydrochloride amount, stirring are stood, layering, separation；Toluene phase and water phase are placed respectively；
2）, at salt workshop section：Step 1）Obtained toluene, which is mutually placed in, to be crystallized into salt oven, and 2mol/L hydrochloric acid is added and stirs into
Salt, the interlayer for crystallizing into salt oven lead to chilled brine cooling, place 1h at -8 DEG C, centrifuge rejection filter after drying, is dried at 70 DEG C
It is dry.
3）, filtrate handle recycle section：By step 2）Caustic lye of soda is added in the filtrate that middle centrifugation filters out and adjusts its PH
It is 7, toluene phase is layered immediately with water phase, and separation mutually concentrates toluene, and concentrate is added 2mol/L hydrochloric acid and is crystallized at salt, rejection filter
Drying is crude product；
4）, refined packing department：Crude product after drying is crushed, is added in a concentration of 25% ethanol solution, dissolving,
Washing, drying, then use pure water, drying, cross 20 mesh screens granulation, temperature be 85 DEG C, negative pressure for 0.1MPA vacuum ring
It is 3 hours dry in border, it crushes, chemical examination, pack.
Embodiment 3
A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, includes the following steps：
1）, dissolution extraction workshop section：Unqualified diphenoxylate hydrochloride and pure water are pressed 1：4 mixing, are sufficiently stirred at 24 DEG C
A concentration of 10% sodium hydroxide solution is added in dissolving, and the pH value for reconciling solution is 9, is filtered after stirring evenly, and mechanical admixture is removed；It will
Filtrate is pumped into extraction kettle, stirs 25min, stands 30min, releases water phase and sets in container, toluene is mutually separately deposited；To the water phase of releasing
It being pumped into extraction kettle after middle addition toluene, toluene amount is 2.5 times of unqualified diphenoxylate hydrochloride amount, and stirring is stood, layering,
Separation will detach toluene obtained and mutually merge twice；Pure water is added in combined toluene phase, the amount of pure water is unqualified
4 times of diphenoxylate hydrochloride amount, stirring are stood, layering, separation；Toluene phase and water phase are placed respectively；
2）, at salt workshop section：Step 1）Obtained toluene, which is mutually placed in, to be crystallized into salt oven, and 2mol/L hydrochloric acid is added and stirs into
Salt, the interlayer for crystallizing into salt oven lead to chilled brine cooling, place 1h at -9 DEG C, centrifuge rejection filter after drying, is dried at 80 DEG C
It is dry.
3）, filtrate handle recycle section：By step 2）Caustic lye of soda is added in the filtrate that middle centrifugation filters out and adjusts its PH
It is 7, toluene phase is layered immediately with water phase, and separation mutually concentrates toluene, and concentrate is added 2mol/L hydrochloric acid and is crystallized at salt, rejection filter
Drying is crude product；
4）, refined packing department：Crude product after drying is crushed, is added in a concentration of 30% ethanol solution, dissolving,
Washing, drying, then use pure water, drying, cross 20 mesh screens granulation, temperature be 80 DEG C, negative pressure for 0.07MPA vacuum ring
It is 4 hours dry in border, it crushes, chemical examination, pack.
Embodiment 4
A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, includes the following steps：
1）, dissolution extraction workshop section：Unqualified diphenoxylate hydrochloride and pure water are pressed 1：4 mixing, are sufficiently stirred at 24 DEG C
A concentration of 10% sodium hydroxide solution is added in dissolving, and the pH value for reconciling solution is 9, is filtered after stirring evenly, and mechanical admixture is removed；It will
Filtrate is pumped into extraction kettle, stirs 20min, stands 25min, releases water phase and sets in container, toluene is mutually separately deposited；To the water phase of releasing
It being pumped into extraction kettle after middle addition toluene, toluene amount is 2.5 times of unqualified diphenoxylate hydrochloride amount, and stirring is stood, layering,
Separation will detach toluene obtained and mutually merge twice；Pure water is added in combined toluene phase, the amount of pure water is unqualified
4.5 times of diphenoxylate hydrochloride amount, stirring are stood, layering, separation；Toluene phase and water phase are placed respectively；
2）, at salt workshop section：Step 1）Obtained toluene, which is mutually placed in, to be crystallized into salt oven, and 2mol/L hydrochloric acid is added and stirs into
Salt, the interlayer for crystallizing into salt oven lead to chilled brine cooling, 1.5h, centrifuge rejection filter, after drying, at 60 DEG C are placed at -10 DEG C
Drying.
3）, filtrate handle recycle section：By step 2）Caustic lye of soda is added in the filtrate that middle centrifugation filters out and adjusts its PH
It is 7, toluene phase is layered immediately with water phase, and separation mutually concentrates toluene, and concentrate is added 2mol/L hydrochloric acid and is crystallized at salt, rejection filter
Drying is crude product；
4）, refined packing department：Crude product after drying is crushed, is added in a concentration of 25% ethanol solution, dissolving,
Washing, drying, then use pure water, drying, cross 20 mesh screens granulation, temperature be 90 DEG C, negative pressure for 0.08MPA vacuum ring
It is 4 hours dry in border, it crushes, chemical examination, pack.
Above example is only to the technical solution recorded in the present invention for example, all do not departing from core of the present invention
In the case of make it is simple deformation or modification each fall within protection scope of the present invention.
Claims (3)
1. a kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content, it is characterized in that：Include the following steps：
1）, dissolution extraction workshop section：Unqualified diphenoxylate hydrochloride and pure water are pressed 1：4 mixing, are sufficiently stirred at 23~25 DEG C
A concentration of 10% sodium hydroxide solution is added in dissolving, and the pH value for adjusting solution is 8.5~9.0, is filtered after stirring evenly, and machinery is removed
Impurity；Filtrate is pumped into extraction kettle, using toluene as extractant, 15~25min is stirred, stands 20~30min, water phase is released and sets
In container, toluene is mutually separately deposited；It is pumped into extraction kettle after toluene is added into the water phase of releasing, toluene amount is for unqualified hydrochloric acid fragrant
2~2.5 times of promise ester amount, stirring are stood, layering, separation, will be detached toluene obtained twice and mutually be merged；In combined toluene
Pure water is added in phase, the amount of pure water is 4~4.5 times of unqualified diphenoxylate hydrochloride amount, and stirring is stood, layering, point
From；Toluene phase and water phase are placed respectively；
2）, at salt workshop section：Step 1）Obtained toluene, which is mutually placed in, to be crystallized into salt oven, and 2mol/L hydrochloric acid is added and stirs into salt, and -7
DEG C~-10 DEG C of 1~1.5h of placement, centrifuge rejection filter after drying, crystal salt dry at 50 DEG C~80 DEG C, crude product is made, filter
Liquid is spare；
3）, filtrate handle recycle section：By step 2）It is middle centrifuge sodium hydroxide solution is added in the filtrate that filters out to adjust its pH be
7, toluene phase is layered immediately with water phase, and separation mutually concentrates toluene, and concentrate is added 2mol/L hydrochloric acid and is crystallized at salt, and rejection filter is dried
It does as crude product；
4）, refined packing department：By step 2）With step 3）Crude product after middle drying crushes, and is added to a concentration of 25%~30%
In ethanol solution, dissolving, washing, drying, then use pure water, drying, cross 20 mesh screens granulation, vacuum drying, crush, change
It tests, pack.
2. the recovery processing technique of the unqualified diphenoxylate hydrochloride of content according to claim 1, it is characterized in that：Step 2）
The interlayer for crystallizing into salt oven leads to chilled brine cooling.
3. the recovery processing technique of the unqualified diphenoxylate hydrochloride of content according to claim 1, it is characterized in that：Step 4）
Described in vacuum drying temperature be：80~90 DEG C, negative pressure is 0.07~0.1MPa, and the time is 3~4 hours.
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| CN201410485039.7A CN105503701B (en) | 2014-09-22 | 2014-09-22 | A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content |
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| CN201410485039.7A CN105503701B (en) | 2014-09-22 | 2014-09-22 | A kind of recovery processing technique of the unqualified diphenoxylate hydrochloride of content |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481316A (en) * | 2008-01-07 | 2009-07-15 | 上海浩洲化工有限公司 | Method for refining 3-nitro benzyl amine hydrochlorate |
| CN103040828A (en) * | 2013-01-07 | 2013-04-17 | 常州康普药业有限公司 | Compound diphenoxylate tablet and preparation method thereof |
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2014
- 2014-09-22 CN CN201410485039.7A patent/CN105503701B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481316A (en) * | 2008-01-07 | 2009-07-15 | 上海浩洲化工有限公司 | Method for refining 3-nitro benzyl amine hydrochlorate |
| CN103040828A (en) * | 2013-01-07 | 2013-04-17 | 常州康普药业有限公司 | Compound diphenoxylate tablet and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| P法L HPLC测定复方地芬诺酯片中盐酸地芬酯含量;殷晓建;《蚌埠医药》;19941231;第12卷(第1期);36-37 * |
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