CN102643612A - Saponifiable matter extraction method and saponifiable matter extraction device - Google Patents

Saponifiable matter extraction method and saponifiable matter extraction device Download PDF

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Publication number
CN102643612A
CN102643612A CN2012101223440A CN201210122344A CN102643612A CN 102643612 A CN102643612 A CN 102643612A CN 2012101223440 A CN2012101223440 A CN 2012101223440A CN 201210122344 A CN201210122344 A CN 201210122344A CN 102643612 A CN102643612 A CN 102643612A
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China
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saponified
black liquor
groove
liquor groove
saponifiable
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CN2012101223440A
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CN102643612B (en
Inventor
吴健
罗劲松
朱远征
汤秋南
徐应盛
黄百文
张贺雨
党佩
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Hunan Jun Thai New Materials Technology Co. Ltd.
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Hu'nan Juntai Pulp Paper Co Ltd
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Abstract

Disclosed are saponifiable matter extraction method and a saponifiable matter extraction device. Saponifiable matters are allowed to stay in a black liquor tank and are extracted from black liquor by separating, and surfactant accounting for 0.2-0.5% of the black liquor by weight or sodium sulfonate accounting for 1%-2% of the black liquor by weight is added in the separating process. The saponifiable matter extraction device comprises the black liquor tank which is provided with at least two saponifiable matter outlets, one saponifiable matter outlet is located at the top of the black liquor tank, other saponifiable matter outlets are lower than the first saponifiable matter outlet and provided with openable gates. The speed of separating and rising of the saponifiable matters can be increased, the time of retention and separation of the saponifiable matters can be adjusted according to production conditions, the saponifiable matters are recycled timely, and accordingly deterioration of the saponifiable matters is prevented, and the extraction rate of the saponifiable matters is increased.

Description

A kind of saponified process for extracting and device thereof
Technical field
The present invention relates to the saponified recovery technology of pulping and papermaking processes field, especially relate to the saponified method of extraction from black liquor; The invention still further relates to the saponified a kind of device of extraction from black liquor.
Background technology
In cork alkaline process process; The resinous acid that disengages with various saponified sodium-salt forms, lipid acid and saponifiable matter not get into vapo(u)rization system after black liquid extraction, it has been reclaimed important economic value; It is fully reclaimed, also help the evaporation operation that alkali reclaims.
Traditional saponified process for extracting, the rare black liquor of slurrying, leave standstill through half concentrated black liquid groove behind finite concentration through evaporation concentration, saponifiedly extract after standing separation at the black liquor groove.A kind of tall oil recovery method is disclosed like CN101392148A; With the pine is in the alkaline process paper process of raw material; Paper pulp is isolated black liquor of pulp making through washing after the boiling, and sending evaporation section to be concentrated into concentration through dehydration by evaporation black liquor is 35~45% half concentrated black liquid, after leaving standstill; The saponified storage tank top that floats in half concentrated black liquid is collected saponified from the top of half concentrated black liquid storage tank.
Because traditional saponified process for extracting receives the influence of saponified separator tank liquid level in the production process bigger; Stop disengaging time and be difficult to reach the ideal state; The saponified in addition speed of from black liquor, separating is lower, and saponified separating effect is undesirable, and saponified extraction yield is low.
Summary of the invention
In order to overcome the defective of prior art, on the one hand, one of technical problem to be solved by this invention provides the saponified process for extracting that a kind of separation efficiency is high, extraction yield is high.
In order to solve the problems of the technologies described above; The present invention provides a kind of saponified process for extracting; Its basic technical scheme is: extract saponified in the black liquor groove, after stopping, from black liquor, the separation, in sepn process, adds the tensio-active agent of black liquor weight 0.2wt%~0.5wt% and/or the sodium sulfate of 1wt%~2wt%.
It is preferably, saponified that in the black liquor groove, to stop separation time be 2.5~3.5 hours.
Preferably, the saponified solid concentration that in the black liquor groove, stops black liquor when separating is 22%~30%.
Preferably, the saponified temperature that in the black liquor groove, stops black liquor when separating is 70~90 ℃.
Further, saponified in the black liquor groove, the stop when separating feeds pressurized air at said black liquor trench bottom and accelerates saponified separation.
Preferably, said tensio-active agent is one or more in X 2073, fatty alcohol polyoxyethylene ether sulfate, secondary alkyl sulfonate, terminal olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester sodium, aliphatic alcohol polyethenoxy ether carboxylate, tea saponin, the polypeptide based surfactants.
On the other hand, one of technical problem to be solved by this invention provides a kind of can the flexible adaptation production process variation, make saponified separation be in the saponified extraction element of preferred process state.
In order to solve the problems of the technologies described above; The present invention provides a kind of saponified extraction element; Its basic technical scheme is: this device comprises the black liquor groove; Said black liquor groove is provided with at least two saponified outlets, and wherein the first saponified outlet is positioned at the top of said black liquor groove, and the installation site of all the other saponified outlets is lower than the said first saponified outlet and all the other saponified outlets are provided with the gate that can open or close.
Further, the black liquor trench bottom of saponified extraction element also has compressed air line and sparger.
Further, the black liquor groove inside of saponified extraction element is provided with and the identical cofferdam of said saponified export volume, and said cofferdam is fixed on black liquor groove inwall, and the outlet of said cofferdam is connected with said saponified outlet.
The beneficial effect that the present invention brings: in saponified stop sepn process, add tensio-active agent, can accelerate saponified separation lift velocity; In saponified stop sepn process, add sodium sulfate, reduced saponified solubleness in black liquor, improve saponified extraction yield; Saponified extraction element is provided with at least two saponified outlets that the installation site height is different; Can be according to the height of the liquid level in the saponified separation black liquor groove; Open the saponified outlet of different heights flexibly,, in time reclaim saponified according to the saponified stop disengaging time of condition of production adjustment; Prevent to cause saponified rottenly, improve saponified extraction yield because of long time stored.
Description of drawings
Below in conjunction with accompanying drawing and embodiment content of the present invention is done further explain:
Fig. 1 is the saponified extraction element master of an embodiment of the invention TV structure synoptic diagram;
Fig. 2 is that A-A of Fig. 1 is to structural representation.
Embodiment
Like Fig. 1, the saponified extraction element of embodiment shown in Figure 2; This device comprises black liquor groove 7, and black liquor groove 7 is provided with two saponified outlets 1 and 3, and wherein the first saponified outlet 1 is positioned at the top of black liquor groove 7; Position and saponified outlet 3 that the installation site of another saponified outlet 3 is lower than the first saponified outlet 1 are provided with the gate 4 that can open or close; Black liquor groove 7 inside are provided with cofferdam 2 and 5, and cofferdam 2 and 5 is fixed on black liquor groove inwall, and the outlet in cofferdam 2 is connected with the first saponified outlet 1; The outlet in cofferdam 5 is connected with saponified outlet 3, and the bottom of black liquor groove 7 also has compressed air line 8 and sparger 6.
Embodiment 1: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 75 ℃, and black liquor solid concentration is 24% black liquor; Be sent in the black liquor groove 7, in this black liquor, add black liquor amount 0.2wt% X 2073 tensio-active agent, in stopping sepn process, also feed pressurized air to the bottom of black liquor groove 7 from compressed air line 8 and sparger 6; Accelerate saponified separation; This black liquor stopped in black liquor groove 7 after 3.5 hours, and partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 2: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 85 ℃, and black liquor solid concentration is 27% black liquor; Be sent in the black liquor groove 7, in this black liquor, add the polypeptide based surfactants of black liquor amount 0.5wt%, in stopping sepn process, also feed pressurized air to the bottom of black liquor groove 7 from compressed air line 8 and sparger 6; Accelerate saponified separation; This black liquor stopped in black liquor groove 7 after 2.5 hours, and partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 3: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 84 ℃, and black liquor solid concentration is 27.5% black liquor; Be sent in the black liquor groove 7, in this black liquor, add the terminal olefin sodium sulfonate tensio-active agent of black liquor amount 0.35wt%, in stopping sepn process, also feed pressurized air to the bottom of black liquor groove 7 from compressed air line 8 and sparger 6; Accelerate saponified separation; This black liquor stopped in black liquor groove 7 after 3 hours, and partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 4: use aforementioned saponified extraction element to extract when saponified; The black liquor that the slurrying extraction obtains is concentrated to temperature in evaporative process be 70 ℃, and black liquor solid concentration is 22% black liquor, is sent in the black liquor groove 7; The sodium sulfate that in this black liquor, adds black liquor amount 0.2wt% fatty alcohol polyoxyethylene ether sulfate tensio-active agent and 1wt%; This black liquor stopped in black liquor groove 7 after 3.2 hours, and partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 5 from saponified outlet 3 outflows through the cofferdam, thereby obtain saponified.
Embodiment 5: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 80 ℃, and black liquor solid concentration is 26% black liquor; Be sent in the black liquor groove 7, in this black liquor, add the sodium sulfate of black liquor amount 2wt%, this black liquor stops after 3.5 hours in black liquor groove 7; Partly-hydrolysed thing is wherein analysed day; Rise to the top of black liquor groove 7,2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Embodiment 6: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 90 ℃, and black liquor solid concentration is 30% black liquor; Be sent in the black liquor groove 7, in this black liquor, add the sodium sulfate of black liquor amount 1.5wt%, in stopping sepn process, also feed pressurized air to the bottom of black liquor groove 7 from compressed air line 8 and sparger 6; Accelerate saponified separation; This black liquor stopped in black liquor groove 7 after 2.6 hours, and partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 5 from saponified outlet 3 outflows through the cofferdam, thereby obtain saponified.
Comparative Examples 7: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 65 ℃, and black liquor solid concentration is 20% black liquor; Be sent in the black liquor groove 7; In black liquor groove 7, stop after 2.2 hours, partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Comparative Examples 8: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 95 ℃, and black liquor solid concentration is 32% black liquor; Be sent in the black liquor groove 7; In black liquor groove 7, stop after 4 hours, partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Comparative Examples 9: use aforementioned saponified extraction element to extract when saponified, the black liquor that obtains is extracted in slurrying, and in evaporative process, to be concentrated to temperature be 68 ℃, and black liquor solid concentration is 35% black liquor; Be sent in the black liquor groove 7; In black liquor groove 7, stop after 5 hours, partly-hydrolysed thing is wherein analysed day, rises to the top of black liquor groove 7; 2 from first saponified outlet 1 outflow through the cofferdam, thereby obtain saponified.
Through to above embodiment or Comparative Examples test, when producing the Pinus massoniana Lamb sulfate pulping, Tall oil quantity such as following table that the ton slurry reclaims from saponified:
Embodiment Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5 Embodiment 6 Comparative Examples 7 Comparative Examples 8 Comparative Examples 9
Ton slurry Tall oil reclaims quantity kg 31.21 32.07 32.41 30.02 31.76 31.23 19.13 26.32 25.18
Test result shows that also the saponified solid concentration that in the black liquor groove, stops black liquor when separating is, can reclaim more Tall oil at 22%~30% o'clock, and concentration reduces or raises, and the yield of Tall oil will reduce; When not adding tensio-active agent or using pressurized air; Saponified in the black liquor groove, the stop when separation time reaches 3.5 hours still can not fully be separated; If it is fully separated; Black liquor need have less liquid-column height when stopping, add tensio-active agent or use pressurized air to help accelerating saponified separation; Add sodium sulfate and help improving saponified yld.
The tensio-active agent that adds can be in X 2073, fatty alcohol polyoxyethylene ether sulfate, secondary alkyl sulfonate, terminal olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester sodium, aliphatic alcohol polyethenoxy ether carboxylate, tea saponin, the polypeptide based surfactants one or more.Can also be quaternized thing, glycerin fatty acid ester etc.
The above is merely the preferred embodiments of the present invention, and does not limit the present invention in any way, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. saponified process for extracting saponifiedly separates from black liquor and extracts through stopping the back in the black liquor groove, it is characterized in that: the tensio-active agent of adding black liquor weight 0.2wt%~0.5wt% and/or the sodium sulfate of 1wt%~2wt% in sepn process.
2. saponified process for extracting according to claim 1 is characterized in that: said saponified in the black liquor groove, to stop separation time be 2.5~3.5 hours.
3. saponified process for extracting according to claim 1 is characterized in that: the said saponified solid concentration that in the black liquor groove, stops black liquor when separating is 22%~30%.
4. saponified process for extracting according to claim 1 is characterized in that: the said saponified temperature that in the black liquor groove, stops black liquor when separating is 70~90 ℃.
5. saponified process for extracting according to claim 1 is characterized in that: said saponified in the black liquor groove, the stop when separating feeds pressurized air at said black liquor trench bottom and accelerates saponified separation.
6. saponified process for extracting according to claim 1 is characterized in that: said tensio-active agent is one or more in X 2073, fatty alcohol polyoxyethylene ether sulfate, secondary alkyl sulfonate, terminal olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester sodium, aliphatic alcohol polyethenoxy ether carboxylate, tea saponin, the polypeptide based surfactants.
7. saponified extraction element that saponified process for extracting according to claim 1 adopted; This device comprises the black liquor groove; It is characterized in that: said black liquor groove is provided with at least two saponified outlets; Wherein the first saponified outlet is positioned at the top of said black liquor groove, and the installation site of all the other saponified outlets is lower than the said first saponified outlet and all the other saponified outlets are provided with the gate that can open or close.
8. saponified extraction element according to claim 7 is characterized in that: said black liquor trench bottom also has compressed air line and sparger.
9. saponified extraction element according to claim 7 is characterized in that: said black liquor groove inside is provided with and the identical cofferdam of said saponified export volume, and said cofferdam is fixed on black liquor groove inwall, and the outlet of said cofferdam is connected with said saponified outlet.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102852021A (en) * 2012-09-11 2013-01-02 长沙理工大学 Black liquor tank used in saponification product extraction, and saponification product extraction method
CN103357194A (en) * 2013-06-14 2013-10-23 武汉轻工大学 Extraction agent for synchronous production of various functional components of cape jasmine, and extraction and separation method thereof
CN106049151A (en) * 2016-08-22 2016-10-26 怀化市双阳林化有限公司 Apparatus and method for separating black liquor from saponified product

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JP2010516872A (en) * 2007-01-26 2010-05-20 ナルコ カンパニー Additives to increase the separation yield of tall oil soap from black liquor

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102852021A (en) * 2012-09-11 2013-01-02 长沙理工大学 Black liquor tank used in saponification product extraction, and saponification product extraction method
CN103357194A (en) * 2013-06-14 2013-10-23 武汉轻工大学 Extraction agent for synchronous production of various functional components of cape jasmine, and extraction and separation method thereof
CN103357194B (en) * 2013-06-14 2016-02-17 武汉轻工大学 The extractant of synchronous production cape jasmine multiple efficacies component and Extraction and isolation method thereof
CN106049151A (en) * 2016-08-22 2016-10-26 怀化市双阳林化有限公司 Apparatus and method for separating black liquor from saponified product

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Address after: 418005 Huaihua Industrial Park, Hunan, Huaihua

Patentee after: Hunan Jun Thai New Materials Technology Co. Ltd.

Address before: 418005 Huaihua Industrial Park, Hunan, Huaihua

Patentee before: Hu'nan Juntai Pulp Paper Co., Ltd.