CN100412151C

CN100412151C - Method for producing colophony by using natural turpentine and residue and waste liquor from colophony production factory

Info

Publication number: CN100412151C
Application number: CNB2006100188232A
Authority: CN
Inventors: 古远亮
Original assignee: Individual
Current assignee: Individual
Priority date: 2006-04-17
Filing date: 2006-04-17
Publication date: 2008-08-20
Anticipated expiration: 2026-04-17
Also published as: CN1837309A

Abstract

The present invention discloses a method for producing colophony by using natural turpentine, and residues and waste liquor from a colophony production factory. The present invention adopts a steaming method which comprises dissolving, coarse filtration, standing, clarification, filtration and distillation of waste slag, distillation of filter liquor and package of finished products. The present invention has the advantage that the effective ingredient yield of the colophony which is produced according to the process method can reach to more than 90 %. On the basis of a common colophony processing technology, the method increases the use level of dissolving oil (turpentine), an inner bag type filter device is additionally arranged in a common dissolving pan, and a standing step of filter liquor is additionally increased in the whole process flow. Thus, the purpose of quickly separating impurities is achieved.

Description

A kind of natural pine gum and rosin factory residue waste liquid of utilizing produced the rosiny method

Technical field

The present invention relates to a kind of rosiny production method, especially a kind of residue waste liquid production rosiny method of utilizing in natural pine gum and the rosin production.

Background technology

Rosin is resinous acid and terebinthine mixture, is water white thick liquid during at first from the outflow of tree body.At present, employing is manually gathered the way of rosin and is obtained, and is processed into rosin and turps then, becomes important chemical material.Artificial its working method of rosin of gathering has steaming process and two kinds of the methods of dripping.Steaming process is that the water vapor that produces with steam boiler is a thermal source, with the rosin heating for dissolving, the impurity of the big grain of filtering is further removed tiny impurity and most moisture content with clarifying method then earlier, should make liquid only at last and in distillation tower, steam turps, and obtain rosin with superheated vapour.The method of dripping rosin processing be at the bottom of still pot directly with coal, firewood heating, splash into clear water, make the profit vaporization of being heated steam turps, and the liquid of staying the bottom of a pan emit filter cooling after, solid rosin.Pinus seeds such as pinus yunnanensis, slash pine, Pinus massoniana Lamb, pinus khasys are endangered by the disease worm, and xylem sustains damage, and wound can flow out a lot of rosin, and these rosin accumulate over a long period, and gather the pine tree root, we this rosin in fallen rosin.This rosin is along with increasing duration of contact with air, turps constantly volatilizees, the solid of yellowing, brown or black, because of this rosin severe oxidation, the foreign matter content height, its physico-chemical property and fresh rosin have tangible difference, so take present conventional rosin production method can't produce the rosin product smoothly.When directly fire drips the production of method rosin, be to filter foreign material with 60～180 purpose metallic sieves, these cross filter residue except that bark, leaf, earth, sandstone, still contain 50～65% rosin, but because of bits are direct-fired products, it local superheating occurs and the phenomenon of burning rosin easily in heat-processed, the oxide content height, normally it is abandoned or incinerates, still do not have at present and utilize it to produce the rosiny report.When steaming process rosin is produced, in the clarification operation, discharge tiny suspended substance (middle level fat liquid), its proportion is between water and fat liquid, but its ratio that contains rosin turpentine reaches 50～70%, as it being recycled, be difficult in that the way with continuous sedimentation obtains clean fat liquid in the placed in-line clarifying kettle group, more can't natural filtration.Normally its collection is accumulated direct heating and temper, simple filtration becomes black rosin to sell, and utility value is extremely low.The denominator of above-mentioned three kinds of raw materials is: the oxide content height, the foreign matter content height is 7～10 times of artificial rosin foreign matter content.Process these three kinds of rosin raw materials and all can not reach the ideal effect: 1 by common artificial rosin working method, artificial rosin is in the heating for dissolving operation, normally add the turps that accounts for raw material weight 15%～25% and make dissolution with solvents rosin, and these three kinds of raw materials are serious because of its oxidation, a small amount of turps can not be with its oxide dissolution or dilution, after being heated, resene becomes a kind of extreme heavy-gravity black jelly, the ratio of this jelly is great, be deposited in device bottom, can influence heat conduction when producing with the method for dripping, lead to the consequence of burning the bottom of a pan, can give life when serious, property brings injury and loss.Promptly the sieve plate of equipment can be clung with steaming process production, line clogging very easily leads to security incident.2, the oxidation rosin back agglutination of being heated because this jelly ventilation property is poor, adheres to each other with bark impurity silt again when dissolving, can not separate with impurity easily, contains a lot of effective ingredients in the filter residue and is dropped, and the product yield is extremely low.3, the defecation scum thing (middle level fat liquid) during steaming process rosin is produced is a kind of suspended substance, and proportion is difficult to common clarification way its suspended substance be separated between water and fat liquid.4, with the way of simple and easy heating processing middle level fat liquid, its product does not have quality index can be sayed, rosin, the terebinthine rate of recovery are extremely low, and it is very big, greatly dangerous to process filtering difficulty simultaneously.

Summary of the invention

The object of the present invention is to provide a kind of fallen rosin and rosin factory residue waste liquid of utilizing to produce the rosiny method, this method has solved an above-mentioned difficult problem.

Technical scheme of the present invention is: a kind of fallen rosin and rosin factory residue waste liquid of utilizing produced the rosiny method, dissolving, coarse filtration: with raw material and solvent, in-5 ℃～120 ℃ temperature range, dissolve, then the thick slag of elimination, and distill thick slag, reclaim solvent; Leave standstill: import several through the filtrate of coarse filtration and leave standstill in the pot, left standstill 40～60 minutes, the most of moisture content slag of venting thing; Clarification: leave standstill filtrate and enter placed in-line clarifying kettle group, clarified 6～8 hours, isolate clean filtrate and precipitation slag thing; Filter, the distillation filter residue: use the centrifugal filter filtering precipitate, and filter residue is imported still pot add thermal distillation, reclaim solvent discharge waste residue, filtrate is returned dissolution process; Distillation fat liquid: the clean filtrate that after clarification, obtains, deliver to distillation in the still pot, reclaim solvent; Packing: after the solvent distillation in the filtrate was reclaimed and finished, the still raffinate was the rosin finished product, and directly the discharging packing is cooled off; It is characterized in that: the solvent in dissolution process is the turps of 0.3～1.5 times of raw material weight.Leaving standstill operation leaves standstill in the pot and leaves standstill for sending into 2～6 after material dissolution is filtered sequentially respectively.In common rosin dissolving pan, increase netted container of a liner type or netted isolation board device, to reach quick filtering purpose.The solvent that adds in dissolution process can replace with gasoline, can also be gasoline and turps, dimethylbenzene and turps, and stump light and terebinthine mixing liquid, its proportioning is 1: 99.

The invention has the advantages that: increase the turps consumption with dissolving fallen rosin and rosin factory residue waste liquid, make material become rarer lighter liquid, and help filtering and accelerating impurity Cheng Dian, in common rosin dissolving pan, increase netted container or netted dividing plate, can increase the filter plate area like this and leach fat liquid fast, sink to the bottom the phenomenon of stopping up sieve plate to overcome impurity.Also in the common rosin production technique, increase many pots and independently left standstill operation, separating suspension effectively, overcome common continuous sedimentation and the defective of front-to-back effect sedimentation effect, use whizzer filtering-depositing slag thing simultaneously, reclaim effective ingredient, reclaim the turps that residues in the bits with the distillatory method, and then obtain rosin by common colophony processing method distillation filtrate.Its effective component yield reaches more than 90%.

Embodiment

Embodiment 1: a kind of fallen rosin that utilizes is produced the rosiny method, and its step is: (1) dissolving, coarse filtration: at the band sieve plate with have in the dissolving pan of slag-drip opening and liner type filtration unit and carry out.The dissolving pan of at first 0.5 ton of fallen rosin being packed into adds 0.5 ton of turps simultaneously, opens the emptying gate valve of condensation reflux unit, feeds lively atmosphere then, and a pot interior material is heated, and temperature slowly rises to 100 ℃, keeps 10 minutes, closes working steam then.Open the grease outlet gate valve, fat liquid is sent into left standstill pot.Open the working steam valve again and feed working steam the bits that rest on the sieve plate are blown distillation, reclaim turps, blow steam finish after, turn off working steam, when confirming in the pot no pressure, open the slag-drip opening deslagging, and then carry out feeding intake next time.The continuous dosing heating for dissolving leaves standstill pot with the input of fat liquid respectively continuously, leaves standstill pot for many pots; (2) leave standstill: coarse filtration filtrate enters to be left standstill in the pot after leaving standstill 1 hour, opens water discharge valve sequentially, the most of pulp water of venting.(3) clarification and waste residue are handled: gained is left standstill liquid send into placed in-line clarifying kettle group clarification 8 hours, the clean fat liquid after the clarification is sent into test tank and is prepared by quantitatively sending into distillation process.The waste residue that respectively leaves standstill the discharge of pot and clarifying kettle gathers in precipitation slag (the middle level fat liquid) storage tank, treated when a certain amount of, feeding is steam heated to 95 ℃, import the centrifugal filter inner filtration then, filtrate is sent dissolution process back to, and filter residue is sent in the spray steamer of being with sieve plate and slag notch and blown steaming, reclaims turps, after recovery finishes, discharge waste residue.(4) distillation fat liquid: quantitatively (capacity 70%) slowly opened the clean filtrate one-level still pot of packing into and closed vapour and working steam, and be heated to 150 ℃ and turn off working steam, fat liquid input secondary distillation pot, the one-level still pot is feeded once more.Fat liquid continues to add thermal distillation at the secondary distillation pot, and kettle temperature reaches 190 ℃, and turps reclaims that to finish be that tail heats up in a steamer the turps ratio d that weighs ₄ ²⁰0.90-0.92 the time discharging barrelling, be the rosin finished product after the cooling.

Embodiment 2: drip method rosin factory residue of a kind of utilization is produced the rosiny method, and its step is: get 0.5 ton of the method rosin factory residue of dripping, add 0.7 ton in gasoline, be heated to 95 ℃ of dissolvings, all the other steps are with embodiment 1.

Embodiment 3: a kind of steaming process rosin factory waste liquid (middle level fat liquid) processing rosiny method of utilizing, its step is: get 0.8 ton of middle level fat liquid, add turps and be heated to 95 ℃ of dissolvings for 0.6 ton, all the other steps are with embodiment 1.

Embodiment 4: a kind of natural pine gum that utilizes is produced the rosiny method, its step is: get 3 tons of natural pine gums, add 3 tons in gasoline, soak at room temperature obtained fat liquid and slag thing in 12 hours in dissolving tank, and filter residue is sent in the still pot of band sieve plate and slag notch, opened the working steam spray and steamed 10 minutes, when treating in the pot no pressure, open the water discharge valve draining, open slag notch again and slag tap, all the other steps are undertaken by embodiment 1.

Embodiment 5: a kind of natural pine gum that utilizes is produced the rosiny method, and its step is: get 0.5 ton of natural pine gum, add 0.3 ton of dimethylbenzene, 0.2 ton in turps is heated to 95 ℃ of dissolvings, and all the other steps are undertaken by embodiment 1.

Embodiment 6: a kind of fallen rosin that utilizes is produced the rosiny method, and its step is: get 0.5 ton in fallen rosin, add 0.3 ton of stump light, 0.3 ton in turps is heated to 95 ℃ of dissolvings, and all the other steps are undertaken by embodiment 1.

Embodiment 7: a kind of fallen rosin that utilizes is produced the rosiny method, and its step is: get 0.5 ton of natural pine gum, add gasoline 0.2, turps 0.3 is heated to 95 ℃ of dissolvings, and all the other steps are undertaken by embodiment 1.

Claims

1. one kind is utilized fallen rosin and rosin factory residue waste liquid to produce the rosiny method, the steps include: (1) dissolving, coarse filtration: with raw material and solvent, in-5 ℃～120 ℃ temperature range, dissolve, the thick slag of elimination then, and distill thick slag, reclaim solvent, in the rosin dissolving pan, carry out during heating for dissolving; (2) leave standstill: send into 2-6 sequentially respectively through the filtrate of coarse filtration and leave standstill in the pot, left standstill 40～60 minutes, the most of moisture content slag of venting thing; (3) clarification: leave standstill filtrate and enter placed in-line clarifying kettle group, clarified 6～8 hours, isolate clean filtrate and precipitation slag thing; (4) filter, the distillation filter residue: use the centrifugal filter filtering precipitate, and filter residue is imported still pot add thermal distillation, reclaim solvent discharge waste residue, filtrate is returned dissolution process; (5) distillation fat liquid: the clean filtrate that after clarification, obtains, deliver to distillation in the still pot, reclaim solvent; (6) packing: after the solvent distillation in the filtrate was reclaimed and finished, the still raffinate was the rosin finished product, and directly discharging is packed, cooling; Solvent in dissolution process is a raw material weight 0.2-0.5 gasoline doubly.

2. a kind of fallen rosin and rosin factory residue waste liquid of utilizing according to claim 1 produced the rosiny method, it is characterized in that: the heating for dissolving in the step 1 is carried out in the rosin dissolving pan, increase netted container of a liner type or netted isolation board device in the rosin dissolving pan, increase the filter plate area, to reach quick filtering purpose.