CN107501030A - Chromatogram pure toluene and preparation method thereof, production system - Google Patents
Chromatogram pure toluene and preparation method thereof, production system Download PDFInfo
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- CN107501030A CN107501030A CN201710756017.3A CN201710756017A CN107501030A CN 107501030 A CN107501030 A CN 107501030A CN 201710756017 A CN201710756017 A CN 201710756017A CN 107501030 A CN107501030 A CN 107501030A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
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- C07C7/005—Processes comprising at least two steps in series
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Abstract
A kind of chromatogram pure toluene and preparation method thereof, production system, it is related to chemical products technical field of purification, the preparation method of chromatogram pure toluene is using the toluene of technical grade as raw material, is firstly added the concentrated sulfuric acid and is reacted, adds sodium acid carbonate neutralization, next is washed, afterwards by 4A molecular sieve adsorptions, it is subsequently added into phosphorus pentoxide and carries out rectifying, the preparation method production cost is low, obtained chromatogram pure toluene quality better, yield are high, meet chromatographically pure reagent requirement.The production system of chromatogram pure toluene includes retort, 4A molecular sieve columns, reactor, rectifying column, finished pot; wherein; retort is connected with 4A molecular sieve columns; retort, reactor, rectifying column, finished pot are sequentially connected with; the production system realizes the scale industrial production of chromatogram pure toluene dedicated for preparing chromatogram pure toluene.
Description
Technical field
The present invention relates to chemical products technical field of purification, and more particularly to a kind of chromatogram pure toluene and preparation method thereof,
Production system.
Background technology
Chromatographically pure refers to carry out the standard reagent or solvent used during chromatography, its ultraviolet light absorption at low wavelength
Degree under chromatographic condition, the peak of appointed compound can only occur than relatively low, it is impossible to there are impurity peaks, therefore, chromatogram pure reagent
Purity requirement is very high, in addition to the requirement to appointed compound content is very high, also has to impurity contents such as micronic dust therein, moisture
Very high requirement, belong to the category of high purity reagent.At present, domestic chromatographically pure market is mostly that external Reagent Company is monopolized, such as
Merck, Sigma, Fisher, Tedia etc., external Reagent Company's price is high, for the chromatographically pure user of the country, can cause
Cost is too high.Therefore, break monopolization of the foreign technology obstacle to the chromatographically pure technical field in China, establish what China had by oneself
The standardization industry of chromatogram pure reagent has great meaning and effect.
Chromatogram pure toluene is one of conventional liquid chromatogram mobile phase, both at home and abroad it has been reported that the purifying work of a variety of toluene
Skill, purification process mainly include：Including：Decolourize, absorption, rectifying, or decolourize, absorption, rectifying such as are combined at the step, these are pure
The shortcomings that change method is that product purity is not high, is unsatisfactory for scientific research requirements, or yield is not high, cost is too high.
Therefore, it is necessary to a kind of low toluene preparation method of production cost, and using chromatogram pure toluene product made from this method
Matter is good, yield is high, can meet chromatographically pure reagent requirement.
The content of the invention
It is an object of the invention to provide a kind of preparation method of chromatogram pure toluene, the method production cost is low, obtained
Chromatogram pure toluene quality better, yield are high.
Another object of the present invention is to provide a kind of chromatogram pure toluene, its quality better, yield are high, meet chromatogram pure reagent
It is required that.
Another object of the present invention is to provide a kind of production system of chromatogram pure toluene, it is dedicated for preparing chromatographically pure
Toluene, realize the scale industrial production of chromatogram pure toluene.
The present invention is solved its technical problem and realized using following technical scheme.
The present invention proposes a kind of preparation method of chromatogram pure toluene, and it comprises the following steps：
Using the toluene of technical grade as raw material, it is firstly added the concentrated sulfuric acid and is reacted, add sodium acid carbonate neutralization, secondly
Washed, afterwards by 4A molecular sieve adsorptions, be subsequently added into phosphorus pentoxide and carry out rectifying.
Further, in present pre-ferred embodiments, adding the specific method that the concentrated sulfuric acid is reacted is：In toluene
The volume ratio of the dropwise addition concentrated sulfuric acid, toluene and the concentrated sulfuric acid is 1~50：2~50, and circular response 2~3 hours below 30 DEG C.
Further, in present pre-ferred embodiments, adding the specific method that sodium acid carbonate neutralizes is：Adding dense sulphur
Sodium acid carbonate is added in solution obtained by acid reaction, circular response 1~2 hour, reacts the gas of generation after charcoal absorption
Discharge.
Further, in present pre-ferred embodiments, the specific method of washing is：In adding sodium acid carbonate and after
Add water in solution, the volume ratio of solution and water is 5~3000：1~50, circulation washing 1~2 hour, 3~4 hours are stood, row
Go out the water layer of lower floor, add water, and circulate washing 1~2 hour, stand 3~4 hours, discharge the water layer of lower floor.
Further, in present pre-ferred embodiments, the specific method by 4A molecular sieve adsorptions is：Will washing gained
Solution circulation be passed through in 4A molecular sieve columns and carry out circulation absorption, flow velocity 0.1~2m/s of the control solution in 4A molecular sieve columns,
16~36 hours circulation time.
Further, in present pre-ferred embodiments, adding phosphorus pentoxide and carrying out the specific method of rectifying is：
Add phosphorus pentoxide in the solution after by 4A molecular sieve adsorptions, the amount ratio of solution and phosphorus pentoxide for 5~
3000L：10~2000g, and heating rectifying is carried out, caused gas passes through rectifying column, establishes infinite reflux, and infinite reflux 3~4 is small
When, start to produce, the certified products of extraction are finished product.
Further, in present pre-ferred embodiments, preparation method is additionally included in ion exchange, the mistake carried out after rectifying
Filter step.
A kind of chromatogram pure toluene, it uses the preparation method of chromatogram pure toluene described above to be made.
A kind of production system of chromatogram pure toluene, it includes：
Retort, the container for neutralizing, being washed for sodium acid carbonate to be reacted, added as the addition concentrated sulfuric acid；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorptions；
Reactor, rectifying column, for adding phosphorus pentoxide and carrying out rectifying；And
Finished pot, for collecting finished product,
Wherein, retort is connected with 4A molecular sieve columns, and retort, reactor, rectifying column, finished pot are sequentially connected with.
Further, in present pre-ferred embodiments, production system also includes being installed on retort and 4A molecular sieve columns
Between circulating pump, form the circulation for carrying out circular response between the top of the bottom of retort, circulating pump and retort
Pipeline, the circulation line for carrying out circulation absorption is formed between retort, circulating pump and 4A molecular sieve columns.
Chromatogram pure toluene of the embodiment of the present invention and preparation method thereof, the beneficial effect of production system are：The present invention is implemented
The preparation method of the chromatogram pure toluene of example is using the toluene of technical grade as raw material, is firstly added the concentrated sulfuric acid and is reacted, then adds
Enter sodium acid carbonate neutralization, next is washed, and afterwards by 4A molecular sieve adsorptions, is subsequently added into phosphorus pentoxide and is carried out essence
Evaporate, the preparation method production cost is low, and obtained chromatogram pure toluene quality better, yield are high, meet chromatographically pure reagent requirement.This hair
The production system of the chromatogram pure toluene of bright embodiment includes retort, 4A molecular sieve columns, reactor, rectifying column, finished pot, its
In, retort is connected with 4A molecular sieve columns, and retort, reactor, rectifying column, finished pot are sequentially connected with, and the production system is special
For preparing chromatogram pure toluene, the scale industrial production of chromatogram pure toluene is realized.
Brief description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below by embodiment it is required use it is attached
Figure is briefly described, it will be appreciated that the following drawings illustrate only certain embodiments of the present invention, therefore be not construed as pair
The restriction of scope, for those of ordinary skill in the art, on the premise of not paying creative work, can also be according to this
A little accompanying drawings obtain other related accompanying drawings.
Fig. 1 is the structural representation of the production system of chromatogram pure toluene provided in an embodiment of the present invention.
Icon：100- production systems；001- feedstock transportation pumps；002- retort；003- regards cup；004- circulating pumps；005-
Blender；006- deep freezers；007-4A molecular sieve columns；008- dropping tanks；009- active carbon adsorption columns；010- reactors；011-
Rectifying column；012- condensers；013- return tanks；014- finished pots；015- finished product delivery pumps；016- cation exchange columns；017-
Filter.
Embodiment
, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical scheme be clearly and completely described.Unreceipted actual conditions person, builds according to normal condition or manufacturer in embodiment
The condition of view is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional production that can be obtained by commercially available purchase
Product.
Chromatogram pure toluene of the embodiment of the present invention and preparation method thereof, production system are specifically described below.
A kind of preparation method of chromatogram pure toluene of the embodiment of the present invention, it comprises the following steps：The toluene of technical grade is made
For raw material, it is firstly added the concentrated sulfuric acid and is reacted, adds sodium acid carbonate neutralization, next is washed, and passes through 4A molecules afterwards
Sieve absorption, is subsequently added into phosphorus pentoxide and carries out rectifying, is preferably also included in the ion exchange carried out after rectifying, filtering step
Suddenly.In the present embodiment, the preparation method of chromatogram pure toluene specifically includes following steps：
S1, the addition concentrated sulfuric acid are reacted：It is added dropwise the concentrated sulfuric acid in toluene, the volume ratio of toluene and the concentrated sulfuric acid is 1~50：
2~50, and circular response 2~3 hours below 30 DEG C.
S2, add sodium acid carbonate neutralization：Sodium acid carbonate, circular response are added in the solution obtained by strong sulfuric acid response is added
1~2 hour, the gas for reacting generation discharged after charcoal absorption.
S3, washing：In adding sodium acid carbonate and after solution in add water, the volume ratio of solution and water is 5~3000：
1~50, circulation washing 1~2 hour, 3~4 hours are stood, the water layer of lower floor is discharged, adds water, and it is small to circulate washing 1~2
When, 3~4 hours are stood, discharges the water layer of lower floor.
S4, pass through 4A molecular sieve adsorptions：The solution circulation for washing gained is passed through in 4A molecular sieve columns and carries out circulation absorption,
Control flow velocity 0.1~2m/s of the solution in 4A molecular sieve columns, 16~36 hours circulation time.
S5, add phosphorus pentoxide and carry out rectifying：Five oxidations two are added in the solution after by 4A molecular sieve adsorptions
The amount ratio of phosphorus, solution and phosphorus pentoxide is 5~3000L：10~2000g, and heating rectifying is carried out, caused gas passes through
Rectifying column, infinite reflux is established, infinite reflux 3~4 hours, starts to produce, the certified products of extraction are finished product.
S6, ion exchange：Solution (i.e. finished product) obtained by rectifying is subjected to ion exchange by cation exchange column.
S7, filtering：Solution obtained by ion exchange is filtered by filter, bottles, produces chromatogram pure toluene.This
In embodiment, filter is 200nm filters.
The embodiment of the present invention provides a kind of chromatogram pure toluene, and it uses the preparation method of above-mentioned chromatogram pure toluene to be made.
Shown in Figure 1, the embodiment of the present invention provides a kind of production system 100 of chromatogram pure toluene, and it includes：For making
Reacted to add the concentrated sulfuric acid, add sodium acid carbonate neutralization, the retort 002 for the container washed；For carrying out 4A points
The 4A molecular sieve columns 007 of son sieve absorption；For adding phosphorus pentoxide and carrying out the reactor 010 of rectifying, rectifying column 011；With
In the finished pot 014 for collecting finished product；For carrying out the cation exchange column 016 of ion exchange；And the mistake for being filtered
Filter 017, wherein, retort 002 is connected with 4A molecular sieve columns 007, retort 002, reactor 010, rectifying column 011, finished product
Tank 014, cation exchange column 016, filter 017 are sequentially connected with.
Wherein, what is filled in 4A molecular sieve columns 007 is activating and regenerating type 4A molecular sieves；The height of rectifying column 011 be 2m~
30m, internal diameter are 4cm~220cm, load glass spring filler, the western tower ring of stainless steel, stainless steel structured packing and ceramics in tower and fill out
At least one of material；The model ABD1UPW3EH1+IDO10-PFA-3/4 300 of cation exchange column 016016；Filter
017017 is 200nm filters 017, its model FLHF20010M3F300+IDO10-PFA-3/4 300, filter 017017
Material is virgin pp or pure polytetrafluoroethylene (PTFE).
In the present embodiment, production system 100 also includes feedstock transportation pump 001 and finished product delivery pump 015, feedstock transportation pump
001 is connected with retort 002, for raw material automatic transport to be entered in retort 002；Finished product delivery pump 015 is installed on finished pot
Between 014 and cation exchange column 016, for the finished product automatic transport in finished pot 014 to be gone out to cation exchange column 016.
In the present embodiment, production system 100 also includes the circulation being installed between retort 002 and 4A molecular sieve columns 007
Pump 004, formed for carrying out following for circular response between the top of the bottom of retort 002, circulating pump 004 and retort 002
Endless tube road, the circulation line for carrying out circulation absorption is formed between retort 002, circulating pump 004 and 4A molecular sieve columns 007.
In the present embodiment, the top of retort 002 is provided with for the dropping tank toward the dropwise addition concentrated sulfuric acid in retort 002
008；The top of retort 002 is provided with the active carbon adsorption column for the gas of reaction generation in adsorption treatment retort 002
009；The bottom of retort 002 is provided with for regarding cup 003 in observing response tank 002；The bottom of retort 002, circulating pump
The blender 005 for being sufficiently mixed solution is provided with the circulation line formed between 004 and the top of retort 002 and is used
In the deep freezer 006 of adjustment control solution temperature, specifically, the bottom of retort 002, regarding cup 003, circulating pump 004, blender
005th, circulation line is formed on the top of deep freezer 006 and retort 002.
In the present embodiment, production system 100 also includes being installed on condenser 012, the return tank 013 at the top of rectifying, rectifying
Tower 011, condenser 012 and return tank 013 form the circulation line for carrying out infinite reflux, fully to carry out rectifying.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The present embodiment provides a kind of chromatogram pure toluene, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method is made：
(1) using the toluene of technical grade as raw material, retort 002 is transported to by feedstock transportation pump 001, it is defeated to close raw material
Pump 001 is sent, open the circulation pump 004, establishes and forms the bottom of retort 002, regarding cup 003, circulating pump 004, blender 005, depth
The circulation line at the top of cooler 006 and retort 002, the valve of the dropping tank 008 equipped with the concentrated sulfuric acid is opened, is started to reaction
The 1500L concentrated sulfuric acids are added dropwise in 1500L toluene in tank 002, keep the temperature in retort 002 to keep circulation below 30 DEG C
Reaction 2.5 hours.
(2) circulation line is kept to work on, the solution into retort 002 (adds molten obtained by strong sulfuric acid response
Liquid) in add with the concentrated sulfuric acid be adapted amount sodium acid carbonate, circular response 1~2 hour, the gas for reacting generation is inhaled through activated carbon
Attached column 009 is emitted into air after adsorbing.
(3) circulation line is kept to work on, the 1500L solution in retort 002 is (after adding sodium acid carbonate neutralization
Solution) in add 25L water, circulation washing 1.5 hours, stop circulation, stand 3.4 hours, by being observed depending on cup 003, discharge
The water layer of lower floor, adds water in retort 002, re-establishes circulation line, circulation washing 1.5 hours, stands 3.5 hours,
Discharge the water layer of lower floor in retort 002.
(4) establish and form retort 002, the circulation line between cup 003, circulating pump 004 and 4A molecular sieve columns 007,
Solution (solution after washing) circulation in retort 002 is passed through in 4A molecular sieve columns 007 and carries out circulation absorption, controls solution
Flow velocity in 4A molecular sieve columns 007 is 1m/s, 24 hours circulation time.
(5) start circulating pump 004, the solution (i.e. by the solution after 4A molecular sieve adsorptions) in retort 002 is passed through
Circulating pump 004,4A molecular sieve columns 007, are delivered into reactor 010, are added in the 1500L solution into reactor 010
1000g phosphorus pentoxides, starting to heat rectifying to the solution in reactor 010, caused gas passes through rectifying column 011, and
Infinite reflux is established between rectifying column 011, condenser 012 and return tank 013, infinite reflux 3.5 hours, starts to produce, removes extraction
Front and rear slop cut, extraction midbarrel certified products (i.e. finished product) are transported to finished pot 014.
(6) start finished product delivery pump 015, the solution (finished product i.e. obtained by rectifying) in finished pot 014 is passed through into cation
Exchange column 016 carries out ion exchange.
(7) solution obtained by ion exchange is filtered by filter 017, bottles, produce chromatogram pure toluene product,
Yield reaches more than 95%.
Embodiment 2
The present embodiment provides a kind of chromatogram pure toluene, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method is made：
(1) using the toluene of technical grade as raw material, retort 002 is transported to by feedstock transportation pump 001, it is defeated to close raw material
Pump 001 is sent, open the circulation pump 004, establishes and forms the bottom of retort 002, regarding cup 003, circulating pump 004, blender 005, depth
The circulation line at the top of cooler 006 and retort 002, the valve of the dropping tank 008 equipped with the concentrated sulfuric acid is opened, is started to reaction
The 500L concentrated sulfuric acids are added dropwise in 1500L toluene in tank 002, keep the temperature in retort 002 below 30 DEG C, keep circulation anti-
Answer 2 hours.
(2) circulation line is kept to work on, the solution into retort 002 (adds molten obtained by strong sulfuric acid response
Liquid) in add with the concentrated sulfuric acid be adapted amount sodium acid carbonate, circular response 1~2 hour, the gas for reacting generation is inhaled through activated carbon
Attached column 009 is emitted into air after adsorbing.
(3) circulation line is kept to work on, the 1500L solution in retort 002 is (after adding sodium acid carbonate neutralization
Solution) in add 5L water, circulation washing 1 hour, stop circulation, stand 3 hours, by being observed depending on cup 003, discharge retort
The water layer of lower floor, adds water in 002, re-establishes circulation line, circulation washing 2 hours, stands 4 hours, discharge retort
The water layer of lower floor in 002.
(4) establish and form retort 002, the circulation line between cup 003, circulating pump 004 and 4A molecular sieve columns 007,
Solution (solution after washing) circulation in retort 002 is passed through in 4A molecular sieve columns 007 and carries out circulation absorption, controls solution
Flow velocity in 4A molecular sieve columns 007 is 2m/s, 36 hours circulation time.
(5) start circulating pump 004, the solution (i.e. by the solution after 4A molecular sieve adsorptions) in retort 002 is passed through
Circulating pump 004,4A molecular sieve columns 007, are delivered into reactor 010, are added in the 1500L solution into reactor 010
2000g phosphorus pentoxides, starting to heat rectifying to the solution in reactor 010, caused gas passes through rectifying column 011, and
Infinite reflux is established between rectifying column 011, condenser 012 and return tank 013, infinite reflux 4 hours, starts to produce, before removing extraction
Slop cut afterwards, extraction midbarrel certified products (i.e. finished product) are transported to finished pot 014.
(6) start finished product delivery pump 015, the solution (finished product i.e. obtained by rectifying) in finished pot 014 is passed through into cation
Exchange column 016 carries out ion exchange.
(7) solution obtained by ion exchange is filtered by filter 017, bottles, produce chromatogram pure toluene product,
Yield reaches more than 95%.
Embodiment 3
The present embodiment provides a kind of chromatogram pure toluene, and it is to use the production system 100 shown in Fig. 1, and according to following
Preparation method is made：
(1) using the toluene of technical grade as raw material, retort 002 is transported to by feedstock transportation pump 001, it is defeated to close raw material
Pump 001 is sent, open the circulation pump 004, establishes and forms the bottom of retort 002, regarding cup 003, circulating pump 004, blender 005, depth
The circulation line at the top of cooler 006 and retort 002, the valve of the dropping tank 008 equipped with the concentrated sulfuric acid is opened, is started to reaction
The 5000L concentrated sulfuric acids are added dropwise in 1500L toluene in tank 002, keep the temperature in retort 002 to keep circulation below 30 DEG C
Reaction 3 hours.
(2) circulation line is kept to work on, the solution into retort 002 (adds molten obtained by strong sulfuric acid response
Liquid) in add with the concentrated sulfuric acid be adapted amount sodium acid carbonate, circular response 1~2 hour, the gas for reacting generation is inhaled through activated carbon
Attached column 009 is emitted into air after adsorbing.
(3) circulation line is kept to work on, the 1500L solution in retort 002 is (after adding sodium acid carbonate neutralization
Solution) in add 50L water, circulation washing 2 hours, stop circulation, stand 4 hours, by being observed depending on cup 003, discharge reaction
The water layer of lower floor, adds water in tank 002, re-establishes circulation line, circulation washing 1 hour, stands 3 hours, discharge reaction
The water layer of lower floor in tank 002.
(4) establish and form retort 002, the circulation line between cup 003, circulating pump 004 and 4A molecular sieve columns 007,
Solution (solution after washing) circulation in retort 002 is passed through in 4A molecular sieve columns 007 and carries out circulation absorption, controls solution
Flow velocity in 4A molecular sieve columns 007 is 0.2m/s, 16 hours circulation time.
(5) start circulating pump 004, the solution (i.e. by the solution after 4A molecular sieve adsorptions) in retort 002 is passed through
Circulating pump 004,4A molecular sieve columns 007, are delivered into reactor 010, are added in the 1500L solution into reactor 010
200g phosphorus pentoxides, starting to heat rectifying to the solution in reactor 010, caused gas passes through rectifying column 011, and in essence
Evaporate and infinite reflux is established between tower 011, condenser 012 and return tank 013, infinite reflux 3 hours, start to produce, remove before and after producing
Slop cut, extraction midbarrel certified products (i.e. finished product) are transported to finished pot 014.
(6) start finished product delivery pump 015, the solution (finished product i.e. obtained by rectifying) in finished pot 014 is passed through into cation
Exchange column 016 carries out ion exchange.
(7) solution obtained by ion exchange is filtered by filter 017, bottles, produce chromatogram pure toluene product,
Yield reaches more than 95%.
The chromatogram pure toluene in the embodiment of the present invention is detected below in conjunction with experiment.
The indices requirement of the chromatogram pure toluene of table 1
First, ultraviolet absorptivity detection is carried out to the chromatogram pure toluene in embodiment 1~3, it is as a result as follows：
The ultraviolet absorptivity testing result of the chromatogram pure toluene of table 2
2nd, water content Indexs measure, evaporation residue Indexs measure and pure are carried out to the chromatogram pure toluene in embodiment 1~3
Spend Indexs measure：Water content Indexs measure instrument model：Metrohm 831KF are led in Switzerland ten thousand；Evaporation residue Indexs measure
Instrument：Assay balance, evaporating dish, water bath with thermostatic control evaporation, baking oven；Purity Indexs measure instrument：Agilent 6890
The flame ionization ditector (GC-FID) of gas-chromatography.Testing result is as follows：
Moisture, evaporation residue, the purity detecting result of the chromatogram pure toluene of table 3
It can be seen that by above-mentioned testing result：The property indices of the chromatogram pure toluene of the embodiment of the present invention are substantially better than
Chromatogram pure toluene standard.
In summary, the production cost of the preparation method of the chromatogram pure toluene of the embodiment of the present invention is low, obtained chromatographically pure
Toluene quality better, yield are high, meet chromatographically pure reagent requirement；The production system of the chromatogram pure toluene of the embodiment of the present invention is specially used
In preparing chromatogram pure toluene, the scale industrial production of chromatogram pure toluene is realized.
Embodiments described above is part of the embodiment of the present invention, rather than whole embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the scope of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiment in the present invention, what those of ordinary skill in the art were obtained under the premise of creative work is not made
Every other embodiment, belongs to the scope of protection of the invention.
Claims (10)
1. a kind of preparation method of chromatogram pure toluene, it is characterised in that it comprises the following steps：
Using the toluene of technical grade as raw material, it is firstly added the concentrated sulfuric acid and is reacted, add sodium acid carbonate neutralization, secondly carry out
Washing, afterwards by 4A molecular sieve adsorptions, is subsequently added into phosphorus pentoxide and carries out rectifying.
2. the preparation method of chromatogram pure toluene according to claim 1, it is characterised in that add what the concentrated sulfuric acid was reacted
Specific method is：It is added dropwise the concentrated sulfuric acid in toluene, the volume ratio of the toluene and the concentrated sulfuric acid is 1~50：2~50, and
Less than 30 DEG C circular responses 2~3 hours.
3. the preparation method of chromatogram pure toluene according to claim 1, it is characterised in that add the tool that sodium acid carbonate neutralizes
Body method is：Sodium acid carbonate is added in the solution obtained by strong sulfuric acid response is added, circular response 1~2 hour, reacts generation
Gas discharges after charcoal absorption.
4. the preparation method of chromatogram pure toluene according to claim 1, it is characterised in that the specific method of washing is：
Add in the solution after sodium acid carbonate neutralizes and add water, the volume ratio of the solution and the water is 5~3000：1~50, circulation
Washing 1~2 hour, 3~4 hours are stood, the water layer of lower floor is discharged, adds water, and circulate washing 1~2 hour, stand 3~4
Hour, discharge the water layer of lower floor.
5. the preparation method of chromatogram pure toluene according to claim 1, it is characterised in that pass through the tool of 4A molecular sieve adsorptions
Body method is：The solution circulation for washing gained is passed through in 4A molecular sieve columns and carries out circulation absorption, control solution is in 4A molecular sieves
0.1~2m/s of flow velocity in post, 16~36 hours circulation time.
6. the preparation method of chromatogram pure toluene according to claim 1, it is characterised in that add phosphorus pentoxide, go forward side by side
The specific method of row rectifying is：Add phosphorus pentoxide in the solution after by 4A molecular sieve adsorptions, the solution and described
The amount ratio of phosphorus pentoxide is 5~3000L：10~2000g, and heating rectifying is carried out, caused gas passes through rectifying column, builds
Vertical infinite reflux, infinite reflux 3~4 hours, starts to produce, the certified products of extraction are finished product.
7. the preparation method of chromatogram pure toluene according to claim 1, it is characterised in that the preparation method is additionally included in
The ion exchange that is carried out after rectifying, filtration step.
8. a kind of chromatogram pure toluene, it is characterised in that it uses the chromatogram pure toluene as any one of claim 1 to 7
Preparation method be made.
9. a kind of production system of chromatogram pure toluene, it is characterised in that it includes：
Retort, the container for neutralizing, being washed for sodium acid carbonate to be reacted, added as the addition concentrated sulfuric acid；
4A molecular sieve columns, for carrying out 4A molecular sieve adsorptions；
Reactor, rectifying column, for adding phosphorus pentoxide and carrying out rectifying；And
Finished pot, for collecting finished product,
Wherein, the retort is connected with the 4A molecular sieve columns, the retort, the reactor, the rectifying column, described
Finished pot is sequentially connected with.
10. the production system of chromatogram pure toluene according to claim 9, it is characterised in that the production system also includes
The circulating pump being installed between the retort and the 4A molecular sieve columns, the bottom of the retort, the circulating pump and institute
State and the circulation line for carrying out circular response is formed between the top of retort, the retort, the circulating pump and described
The circulation line for carrying out circulation absorption is formed between 4A molecular sieve columns.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710756017.3A CN107501030A (en) | 2017-08-29 | 2017-08-29 | Chromatogram pure toluene and preparation method thereof, production system |
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| CN201710756017.3A CN107501030A (en) | 2017-08-29 | 2017-08-29 | Chromatogram pure toluene and preparation method thereof, production system |
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| CN102964200A (en) * | 2012-11-26 | 2013-03-13 | 北京旭阳化工技术研究院有限公司 | Purifying method of coking toluene |
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| CN102060650A (en) * | 2010-12-29 | 2011-05-18 | 天津市康科德科技有限公司 | Method for purifying chromatographic grade toluene |
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