A kind of continuous combination reaction of barium sulfate and reaction end automatic detection device and method
Technical field
The present invention relates to chemical production fields more particularly to a kind of continuous combination reaction of barium sulfate and reaction end to examine automatically
Survey device and method.
Background technique
Concentration is mainly 12%-14% barium sulfide solution and concentration 25%--27% sodium sulphate by barium sulfate combination reaction
Solution carries out metathesis reaction in chemical combination tank, generates the reaction process of barium sulfate and vulcanized sodium.Reactional equation is as follows:
BaS+Na2SO4=BaSO4+Na2S,
Domestic main large-scale production enterprise all chemical combination processes all use the intermittent tissue of combination reaction kettle for a long time
Production.The technology produced using serialization symphysis is never made a breakthrough for decades.Causing the basic reason of this situation is
Chemical combination terminal uses always manual discontinuous sample detection, and the continuous endpoint technique that detects fails to obtain breakthrough.Greatly
Limit the application to mechanization, automation and informationization of chemical combination process.
Intermittent reaction, manual inspection terminal method be: to empty reactor tank and meanwhile be added 12% -14% barium sulphide and
With 25%--27% metabisulfite solution, feed while stirring.When being added to the 1/2 of tank internal volume, start to survey terminal by hand.Side
Method is to dip reaction slurry, is filled into two clean test tubes with funnel and qualitative filter paper.Into test tube, lye is added dropwise respectively
10% metabisulfite solution and 10% barium sulfide solution.Whether there is or not white opacity generations for lye in observation test tube.If sodium sulphate is added dropwise
Muddiness is generated, illustrates that barium sulphide is excessive in slurry, then requires supplementation with addition sodium sulphate., whereas if barium sulphide is added dropwise in test tube
There is white opacity, then illustrates sodium sulphate excess, require supplementation with barium sulphide.So reaction addition is found, until being added any one
, there is not muddiness in kind of detection agent, then to be reacted to terminal (being commonly called as " two is clear ").This is the process of a continuous trial and error, until
It adjusts and completes.Often there is material in tank and fills it up with the case where still can not find terminal.
The drawbacks of manual inspection terminal is clearly:
1, charging charging process is similar to " blind operation ", only leans on subsequent manual inspection, and efficiency is very low;
2, the examined personnel's subjective factor of manual inspection and sense of responsibility influence very big, it is difficult to guarantee that every batch of product is all reacted to
Terminal, when reacting end of a period, sodium sulphate is excessive, then akali sulphide product iron ion increases, and color reddens, quality degradation, if
Barium sulphide is excessive, then the barium that dissociates in barium sulfate product severely exceeds, and causes product unqualified;
3, intermittent operation material residence time in each tank is different, and amount of cure is different, the interstitial of product batches
Amount fluctuation is very big;
4, when intermittent operation, due to feeding every time, material is more by few change in tank, and volume of material rises steadily, for one
For the barium sulphide or sodium sulphate charging rate of a fixation, raw material be added tank in moment concentration distribution gradient be in variation,
The variation of concentration distribution gradient brings the variation of reaction speed, and being changed significantly for reaction speed influences the change of barium sulfate product partial size
Change.
In the above-mentioned methods, test and production practices all confirm, in intermittent reaction tank, since raw material is in tank when initial charge
Interior concentration gradient is big, and reaction speed is fast, and partial size is smaller, and as material increases in tank, the raw material liq of constant inflow is by tank
Material stock " dilution ", concentration gradient becomes smaller, and partial size increases.Therefore the barium sulfate product particle diameter distribution that intermittent reaction obtains is wide in range,
Quality is lower.
For a long time this situation fail take on a new look the reason of be:
It 1, is to roast to generate using barite deposit, since barite deposit quality is continuous due to material liquid especially barium sulphide
Fluctuation, roasting condition stability is difficult to absolutely control, therefore barium sulphide content is between 12% -14% always and fluctuates, can not
It is accurately controlled, identical flow cannot be guaranteed barium sulphide stable components therein, this is that operational characteristic determines.Due to sulphur
Change barium solution and be easy fouling, exact level measurement can not be carried out to it using fine instrument;
2, barium sulfate reaction is a reaction process to terminal and its sensitivity, in a 30m3Chemical combination tank in, terminal
At the end of, even if terminal can all shift, and influence product matter in addition 500-800g raw materials (sodium sulphate or barium sulphide)
Amount, the requirement to precision have reached 3/100000ths, have been capable of providing such precision currently without any online monitoring instruments.
Summary of the invention
The purpose of the invention is to overcome the deficiencies in the prior art, a kind of continuous combination reaction of barium sulfate and reaction are obtained
Terminal automatic detection device and method.
The present invention is achieved through the following technical solutions:
A kind of continuous combination reaction of barium sulfate and reaction end automatic detection device, including being sequentially connected in series first together
The bottom of chemical combination tank, the second chemical combination tank, third chemical combination tank and the 4th chemical combination tank, the first chemical combination tank passes through pipeline connection second
The lower part of chemical combination tank side, the top of the second chemical combination tank other side are connected to the top of third chemical combination tank side by pipeline,
The lower part of the third chemical combination tank other side is connected to the lower part of the 4th chemical combination tank side by pipeline, and the 4th chemical combination tank is another
The lower part of side is connected to discharge nozzle, is respectively set in the first chemical combination tank, the second chemical combination tank, third chemical combination tank and the 4th chemical combination tank
There are agitating device and detector, once barium sulfide solution feed pipe and a metabisulfite solution are set on the first chemical combination tank
Feed pipe is provided with post-cure barium solution feed pipe and secondary metabisulfite solution feed pipe on the second chemical combination tank, described
Barium sulfide solution feed pipe, a metabisulfite solution feed pipe, post-cure barium solution feed pipe and two sodium hydrosulfides are molten
Solenoid valve is respectively arranged on liquid feed pipe;
Wherein, the detector includes nutsch filter and vacuum tank, and the nutsch filter is arranged in corresponding chemical combination tank and leads to
It crosses suction filtration pipeline to be connected in vacuum tank, barium sulphide detection pipeline and sodium sulphate detection pipe has been arranged in parallel on the suction filtration pipeline
Road, the barium sulphide detect and are provided with the first glass tube on pipeline, be communicated on first glass tube by solenoid valve
Barium sulphide detects flow container, is provided with the second glass tube on the sodium sulphate detection pipeline, passes through electromagnetism on second glass tube
Regulating valve is communicated with sodium sulphate detection flow container, is also provided with and communicated with vacuum breaker pipe by solenoid valve above the vacuum tank,
Recovery tube is also provided with and communicated with by solenoid valve below the vacuum tank;
Camera is provided on the outside of the detector, the liquid color in corresponding detector is passed through image by the camera
Signal is transmitted to control system so that control system adjusts the folding of corresponding solenoid valve.
The present invention further improvement lies in that, detect pipeline and sodium sulphate in barium sulphide on the suctions filtration pipeline and detect pipeline simultaneously
The front side of interlink point also passes through solenoid valve and is provided with washing pipe.
The present invention further improvement lies in that, 108C ciphering type filter cloth is provided in the nutsch filter.
The present invention further improvement lies in that, the coconnected solenoid valve of the second chemical combination tank is accurate aciculiform electromagnetism tune
Save valve.
The present invention further improvement lies in that, the recovery tube is connected in corresponding chemical combination pipe so that detection liquid can recycle benefit
With.
Further object of the present invention is, a kind of continuous combination reaction of barium sulfate and reaction end automatic testing method are provided,
It is characterized in that, based on the continuous combination reaction of a kind of barium sulfate described above and reaction end automatic detection device, including with
Lower step:
S1, metabisulfite solution and barium sulfide solution are passed through into solenoid valve continuous charging;
S2, chemical combination slurry flow successively through the first chemical combination tank, the second chemical combination tank, third chemical combination tank and the 4th chemical combination tank, and really
It protects after the completion of chemical combination curing in the discharging of the 4th chemical combination tank.
The present invention further improvement lies in that, the step S2 specifically:
Detector in S201, the first chemical combination tank detects the chemical combination slurry in the first chemical combination tank, if first changes
It closes tank to fail to terminal, then finely tunes the additive amount of metabisulfite solution or barium sulfide solution, until the detection in the second chemical combination tank
Device to the chemical combination slurry in the second chemical combination tank carry out test and analyze reach home until;
S202, third chemical combination tank detector in third chemical combination tank chemical combination slurry carry out terminal verification, if do not complete,
Then by the additive amount of solenoid valve accurate adjustment metabisulfite solution or barium sulfide solution in the second chemical combination tank, if completing,
It is discharged by the 4th chemical combination tank.
The present invention, which further improves, to be, the specific steps that the detector is detected are as follows:
A, nutsch filter is inserted into corresponding chemical combination tank, opens vacuum, the sulphur of filtering is continuously extracted from corresponding chemical combination tank
Change sodium filtered fluid;
B, the filtered fluid extracted in step a passes through the first glass tube and the second glass tube respectively, is respectively 6% by concentration
Barium sulphide detection liquid is added drop-wise at a slow speed the first glass tube, the sodium sulphate detection liquid that concentration is 10% is added drop-wise at a slow speed the second glass
Guan Zhong;
C, inlet amount is adjusted until white is not presented in the first glass tube and the second glass tube or to be white, then be anti-
Terminal should be arrived.
The present invention, which further improves, to be, the judgment method that inlet amount is adjusted in the step c is to be seen by camera
The variation for examining liquid color in the first glass tube and the second glass tube, if there is whiting, correspond to chemical combination tank in lack with it is right
The interior identical raw material of detection liquid that is added dropwise of glass tube is answered not lack if transparent and color is constant.
The step of present invention, which further improves, to be, the detector is detected further include:
D, detector continuous work for a period of time after, by vacuum tube breaking vacuum, recovered material enters corresponding chemical combination tank
Interior recycling;
E, sensors work for a period of time after, open and rinse effective hot water injection's detector, keep nutsch filter, the first glass
Pipe and the second glass tube are pollution-free.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention is able to achieve continuous detection terminal, to create condition for continuous combination reaction, and in production line reality
In the application of border, stable and reliable operation;
2, in the present invention due to combination reaction can continuous operation, concentration distribution gradient is no longer in chemical combination tank for raw material liq
It changes with time, therefore is able to produce out partial size and stablizes, be distributed very narrow barium sulfate product, significant increase product
Quality;
3, continuous end point determination ensures that reaction end without dead angle, has prevented the influence of human subjective's factor in the present invention,
Eliminate product batches difference in quality;
4, chemical combination production and end point determination all realize automation in the present invention, reduce cost of labor, improve production
Efficiency.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of device in the present invention;
Fig. 2 is the enlarged structure schematic diagram of detector in the present invention;
In figure: 1, the first chemical combination tank, the 2, second chemical combination tank, 3, third chemical combination tank, the 4, the 4th chemical combination tank, 5, barium sulphides
Solution feed pipe, 6, metabisulfite solution feed pipes, 7, post-cure barium solution feed pipe, 8, the charging of secondary metabisulfite solution
Pipe, 9, solenoid valve, 10, detector, 101, nutsch filter, 102, vacuum tank, 103, barium sulphide detection pipeline, 104, sodium sulphate
Detection pipeline, the 105, first glass tube, the 106, second glass tube, 107, barium sulphide detection flow container, 108, sodium sulphate detection flow container,
109, vacuum pump, 1010, vacuum breaker pipe, 1011, recovery tube, 1012, washing pipe.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
As shown in Figure 1 to Figure 2, the present invention provides a kind of continuous combination reactions of barium sulfate and reaction end to detect dress automatically
It sets, it is described including being sequentially connected in series the first chemical combination tank 1, the second chemical combination tank 2, third chemical combination tank 3 and the 4th chemical combination tank 4 together
The bottom of first chemical combination tank 1 by pipeline be connected to 2 side of the second chemical combination tank lower part, 2 other side of the second chemical combination tank it is upper
Portion is connected to the top of 3 side of third chemical combination tank by pipeline, and the lower part of 3 other side of third chemical combination tank is connected to the by pipeline
The lower part of four chemical combination tanks, 4 side, the lower part of 4 other side of the 4th chemical combination tank are connected to discharge nozzle, the first chemical combination tank 1, the
Agitating device (diagram does not mark) and detector 10 are respectively arranged in two chemical combination tanks 2, third chemical combination tank 3 and the 4th chemical combination tank 4,
Once barium sulfide solution feed pipe 5 and a metabisulfite solution feed pipe 6 be set on the first chemical combination tank 1, described second
Post-cure barium solution feed pipe 7 and secondary metabisulfite solution feed pipe 8 are provided on chemical combination tank 2, a barium sulphide is molten
5, metabisulfite solution feed pipes 6 of liquid feed pipe, post-cure barium solution feed pipe 7 and secondary metabisulfite solution feed pipe 8
On be respectively arranged with solenoid valve 9;
Wherein, the detector 10 includes nutsch filter 101 and vacuum tank 102, and the nutsch filter 101 is arranged in correspondingization
It closes in tank and is connected in vacuum tank 102 by filtering pipeline, barium sulphide detection pipeline has been arranged in parallel on the suction filtration pipeline
103 and sodium sulphate detect pipeline 104, be provided with the first glass tube 105, first glass on barium sulphide detection pipeline 103
Barium sulphide is communicated with by solenoid valve 9 on glass pipe 105 and detects flow container 107, is provided on the sodium sulphate detection pipeline 104
Second glass tube 106 is communicated with sodium sulphate by solenoid valve 9 on second glass tube 106 and detects flow container 108, described
102 top of vacuum tank is also provided with and communicated with vacuum breaker pipe 1010 by solenoid valve 9, and 102 lower section of vacuum tank also passes through
Solenoid valve 9 is provided with and communicated with recovery tube 1011;
Camera is provided on the outside of the detector 10, the camera passes through the liquid color in corresponding detector 10
Picture signal is transmitted to control system so that control system adjusts the folding of corresponding solenoid valve.
In the above-mentioned technical solutions, pass through the staggered pipeline connection type of setting height, it can be ensured that in corresponding chemical combination tank
The interior chemical combination curing time.
When it is implemented, detecting pipeline 103 and sodium sulphate detection pipeline 104 and interlink in barium sulphide on the suction filtration pipeline
The front side of point also passes through solenoid valve 9 and is provided with washing pipe 1012.
When it is implemented, being provided with 108C ciphering type filter cloth in the nutsch filter 101, it is ensured that filtrate transparency.
When it is implemented, the coconnected solenoid valve 9 of the second chemical combination tank 2 is accurate aciculiform solenoid valve 9.
When it is implemented, the recovery tube 1011 is connected in corresponding chemical combination pipe so that detection liquid can recycle.
Further object of the present invention is, a kind of continuous combination reaction of barium sulfate and reaction end automatic testing method are provided,
It is characterized in that, based on the continuous combination reaction of a kind of barium sulfate described above and reaction end automatic detection device, including with
Lower step:
S1, metabisulfite solution and barium sulfide solution are passed through into 9 continuous charging of solenoid valve;
S2, chemical combination slurry flow successively through the first chemical combination tank 1, the second chemical combination tank 2, third chemical combination tank 3 and the 4th chemical combination tank 4,
And ensure to discharge after the completion of chemical combination curing in the 4th chemical combination tank 4.
The present invention further improvement lies in that, the step S2 specifically:
Detector 10 in S201, the first chemical combination tank 1 detects the chemical combination slurry in the first chemical combination tank 1, if the
One chemical combination tank 1 fails to terminal, then finely tunes the additive amount of metabisulfite solution or barium sulfide solution, until in the second chemical combination tank 2
Detector 10 to the chemical combination slurry in the second chemical combination tank 2 carry out test and analyze reach home until;
S202, third chemical combination tank 3 detector 10 in third chemical combination tank 3 chemical combination slurry carry out terminal verification, if not
It completes, then by the additive amount of 9 accurate adjustment metabisulfite solution of solenoid valve or barium sulfide solution in the second chemical combination tank 2, if
It completes, is then discharged by the 4th chemical combination tank 4.
When it is implemented, the specific steps that the detector 10 is detected are as follows:
A, nutsch filter 101 is inserted into corresponding chemical combination tank, opens vacuum, continuously extract filtering from corresponding chemical combination tank
Vulcanized sodium filtered fluid;
B, the filtered fluid extracted in step a passes through the first glass tube 105 and the second glass tube 106 respectively, respectively by concentration
Detect that liquid is added drop-wise at a slow speed the first glass tube 105, the sodium sulphate that by concentration is 10% detects liquid and is added dropwise at a slow speed for 6% barium sulphide
Into the second glass tube 106;
C, inlet amount is adjusted until white is not presented in the first glass tube 105 and the second glass tube 106 or for white,
It is then to be reacted to terminal.
When it is implemented, the judgment method for adjusting inlet amount in the step c is, the first glass tube is observed by camera
105 and second the variation of liquid color in glass tube 106 correspond to and lack in chemical combination tank and corresponding glass if there is whiting
The identical raw material of detection liquid is added dropwise in pipe not lack if transparent and color is constant.
When it is implemented, the step of detector 10 is detected further include:
D, 10 continuous work of detector for a period of time after, by vacuum tube breaking vacuum, recovered material enters corresponding chemical combination
It is recycled in tank;
E, detector 10 after a period of work, is opened and rinses effective hot water injection's detector 10, holding nutsch filter 101,
First glass tube 105 and the second glass tube 106 are pollution-free.
In the above-mentioned technical solutions, barium sulfate, which generates, reacts very sensitive to reaction end, even if using precision 0.01%
Instrument be not still able to satisfy reaction require.Lack end point determination instrument at present, also lacks sulfate ion, barium ions, sulphur grain
The on-line quick detection means of son and sodium particle.In 30 cubic metres of chemical combination tanks, after the reaction was completed, even if adding 1-2Kg sulphur more
Sour sodium or barium sulphide, terminal can all deviate, and therefore, the color change that filtrate after detecting liquid is added by observation is that detection is reacted eventually
The most reliable method of point.Multiple groups camera is set, whole imaging is carried out to the 10 glass tube position of detector in corresponding chemical combination tank,
Teletransmission can be realized unattended to production line to Central Control Room.Remote operating system, modification and fine tuning chemical combination tank are used simultaneously
The full-automation of chemical combination process may be implemented in inlet amount.
Embodiment:
It 1, is 25m by capacity3The first chemical combination tank 1, the second chemical combination tank 2, third chemical combination tank 3 and the 4th chemical combination tank 4, successively
It is cascaded, is fed by the first chemical combination tank 1, glass is all set in the first chemical combination tank 1, the second chemical combination tank 2 and third chemical combination tank 3
The filtering of glass tube type vacuum detects each 1 set automatically, is provided with sodium sulphate and barium sulphide accurate adjustment pipe, each mother tube in the second chemical combination tank 2
Provided with solenoid valve 9;
2, after feeding, slurry flows successively through the first chemical combination tank 1, the second chemical combination tank 2, third chemical combination tank 3 and the 4th chemical combination tank
4, by the detector 10 in the first chemical combination of camera detection tank 1, the second chemical combination tank 2, third chemical combination tank 3 and the 4th chemical combination tank 4,
1 sodium sulphate of the first chemical combination tank and barium sulphide feed liquid feeding quantity are finely tuned, practical operation proves, does not need generally to fine-tune the second change
The material liquid fine tuning pipe closed on tank 2 can make the detection of the detector 10 on the second chemical combination tank 2 and third chemical combination tank 3 reach " two is clear "
State;
3, the barium sulfate product produced by this covering device, is detected through check analysis, and main indicator is obviously improved, and is shown in Table 1.
Table 1, interval chemical combination manual inspection and the automatic testing product table of comparisons of continuous chemical combination
Upper table explanation, is continuously detected using continuous chemical combination-terminal, and the barium sulfate product particle diameter distribution of acquisition significantly narrows,
Stability is more preferable.Barium sulfate and the free barium of vulcanization alkali product or iron ion content are lower and stable, color yellow-white, and no batch is poor
Not.The barium sulfate particle diameter distribution of intermittent-manual inspection method is wide in range, and barium sulfate and akali sulphide product quality are also unstable,
There is batch difference.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.