Refining method for desulphurizing and deodorizing crude sulphate turpentine

A technology of sulfate turpentine and a refining method, which is applied in the refining field of crude sulfate turpentine, can solve the problems of complicated operation, high cost, large pollution and the like, and achieves the effects of time-saving operation, low cost and high product quality.

Inactive Publication Date: 2010-02-24
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems of cumbersome operation, high cost, poor effect and large pollution in the existing sulfate turpentine refining method, the inventi

Method used

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  • Refining method for desulphurizing and deodorizing crude sulphate turpentine
  • Refining method for desulphurizing and deodorizing crude sulphate turpentine
  • Refining method for desulphurizing and deodorizing crude sulphate turpentine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In 100mL (about 87g) sulfur content, add 2.01g active ingredient content to be 46.5%wt p-menthane hydroperoxide (equivalent to 2.3% of raw material quality, the actual consumption of oxygenant and The ratio of the theoretical value is 1:1.15), stirring, heating to 110°C, and keeping the temperature for 9h;

[0030] Add 150 mL of distilled water to the reaction solution, continue to stir for 10 minutes, let the reaction solution stand for stratification, and remove the aqueous solution; directly carry out steam distillation on the organic layer, and collect the distillate with the outlet temperature of the distillation head at 96°C, 97°C, and 98°C respectively. parts, the resulting volumes were 16.5mL, 15mL, and 49.5mL, respectively, and the remaining residue was 10mL;

[0031] The mass volume fraction (ie content) of sulfur in each fraction and still raffinate was measured with a microcomputer sulfur and chlorine analyzer, and the results were 317.99mg / L, 150.40mg / L, 30...

Embodiment 2

[0035] The proportioning of embodiment 2, 3, reaction conditions and operation method etc. are identical with embodiment 1, just in embodiment 2 and embodiment 3, p-menthane hydroperoxide in embodiment 1 is replaced by pinane hydrogen Peroxide and p-cymene hydroperoxide as reagents for oxidative desulfurization of crude sulfate turpentine.

[0036] The reaction conditions and results of Examples 1-3 are listed in Table 1.

[0037] Table 1 Desulfurization and deodorization reaction conditions and effects of CST

[0038]

[0039] Here, rate of recovery=(volume of fraction volume / raw raw material crude sulfate turpentine collected by distillation)×100

[0040] The raw materials CST used in Examples 1 to 3 are the same, and the amount of oxidizing agent refers to the ratio of the actual amount added to the theoretically calculated amount, where the theoretically calculated amount refers to the amount of oxygen required to completely oxidize the sulfur contained in the raw mate...

Embodiment 4～12

[0043] Embodiment 4~12 is to select oxidant type, oxidant consumption, reaction temperature, reaction time as 4 factors of orthogonal test, then respectively get 3 different values ​​as 3 level values ​​of orthogonal test, respectively correspond to: pair menthane hydroperoxide, H 2 o 2 , Pinane hydroperoxide; 2.8, 2.4, 2.0; 110°C, 100°C, 90°C; 8h, 9h, 10h. which added H 2 o 2 This reaction factor is to compare with the oxidation effect of some oxidizing agents in use today. The reaction conditions and effects of Examples 4-12 are listed in Table 2.

[0044] Table 2 CST desulfurization and deodorization reaction orthogonal test conditions and effects

[0045]

[0046] The results in Table 2 show that this process can greatly reduce the sulfur content in the raw material sulfate turpentine, the minimum can reach below 20mg / L, and hardly feel obvious stench, and the color of turpentine also changes from original yellow to colorless and transparent .

[0047] In terms o...

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Abstract

The invention relates to a refining method for desulphurizing and deodorizing crude sulphate turpentine. The method comprises the following steps: terpene hydroperoxide is taken as oxidation deodorizer, and is added into a reaction bulb with sulphate turpentine which contains sulfur and has putrid odor; the mixture is heated under 50-150 DEG C and is stirred to react for 4-20h; the quantity of oxidation deodorizer added in the reaction accounts for 1%-20% of that of raw material sulphate turpentine, which equals to 0.5-10 times that of theoretical quantity; distilled water is added for washingreaction liquid; water layer is removed by liquid division; organic horizoni is distilled by steam; distillats with different boiling points are segmently collected; and a computer sulfur-chlorine analyzer is utilized to measure the contents of sulfur in each distilled constituent, residue and raw materials, then nearly odorless and colourless refineing sulphate turpentine with the content of sulfur less than or equal to 20mg/l is obtained. The invention combines two processes mutually, namely oxidized desulfurization and deodorization and steam distillation, therefore, no pollutant is generated, and the generated by-product terpene alcohol compound is important spice and emulsifier.

Description

technical field [0001] The invention relates to a method for refining crude sulfate turpentine, in particular to a refining process for removing sulfur-containing organic compounds in crude sulfate turpentine by performing an oxidation reaction with an oxidant and combining with steam distillation. Background technique [0002] Crude sulfate turpentine (usually referred to as CST, which is the acronym for Crude Sulfate Turpentine in English) is a by-product produced during the cooking of wood chips during the kraft pulping process using coniferous wood as raw material. The yellow or dark red oily liquid obtained after the terpenes, sulfides and other gases discharged together with the steam are condensed and cooled and separated from oil and water. The most obvious characteristic of CST is the presence of malodorous sulfur compounds. With the development of my country's paper industry, the output of CST is also increasing. Due to its relatively low cost, it has gradually be...

Claims

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Application Information

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IPC IPC(8): C09F3/02
Inventor 赵振东王婧毕良武李冬梅陈玉湘古研隋管华
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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