CN104055219B - The method of preparation and the application of the tobacco additive for producing cigarette - Google Patents

The method of preparation and the application of the tobacco additive for producing cigarette Download PDF

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CN104055219B
CN104055219B CN 201410276135 CN201410276135A CN104055219B CN 104055219 B CN104055219 B CN 104055219B CN 201410276135 CN201410276135 CN 201410276135 CN 201410276135 A CN201410276135 A CN 201410276135A CN 104055219 B CN104055219 B CN 104055219B
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CN 201410276135
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CN104055219A (en )
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韩咚林
戴亚
闫立峰
朱立军
谭兰兰
陈琨燕
梁坤
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川渝中烟工业有限责任公司
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Abstract

本发明公开了一种烟丝添加剂的其制备方法以及用于生产卷烟的应用,该烟丝添加剂是由石墨烯氧化物通过超声波分散于水中并得到浓度为0.1wt%~0.3wt%的均相溶液;烟丝添加剂的制备方法,其制备方法步骤:a、低温氧化反应;b、中温氧化反应;c、高温氧化反应;d、离心处理;e、超声波分散;将步骤c得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂;该烟丝添加剂用在生产卷烟上的应用如下:用高压喷雾器将烟丝添加剂均匀喷洒在卷烟的烟丝表面,再进行平衡处理。 The present invention discloses a method for preparing tobacco for the manufacture of the additive and the cigarette, the tobacco additive is dispersed in water and ultrasonic waves to give a concentration of 0.1wt% ~ 0.3wt% of the homogeneous solution through the graphene oxide; prepared tobacco additive preparation method steps: a, the low-temperature oxidation reaction; B, intermediate temperature oxidation reaction; c, high temperature oxidation reaction; D, centrifugation; E, ultrasonic dispersion; step c resulting liquid tobacco additives freeze, after the drying process to obtain a fluffy tobacco additive; tobacco additives in the production of cigarettes following applies: a high pressure sprayer tobacco additive is uniformly sprayed on the surface of the cigarette tobacco, and then balancing process. 本发明有较好的降温效果,其平均降低温度为30~45℃,最大幅度降低卷烟抽吸最高温度79℃;有效地降低了卷烟燃烧的有害物质释放,并且卷烟在燃烧抽吸质量上几乎无变化。 The present invention preferably has a cooling effect, reducing the average temperature is 30 ~ 45 ℃, the most significant reduction in the maximum temperature of the suction cigarette 79 ℃; effectively reduces the release of harmful substances in the cigarette burning, and cigarette smoking quality of combustion in almost No change.

Description

烟竺添加剂的制备方法从及用于生产卷烟的应用 Zhu is prepared as an additive for producing tobacco from cigarettes and

技术领域 FIELD

[0001] 本发明设及卷烟烟丝添加剂技术领域,尤其设及一种烟丝添加剂的其制备方法W 及用于生产卷烟的应用,特别设及一种烟丝添加剂通过溶液喷雾法与卷烟烟丝混合。 [0001] The present invention is provided and cut tobacco additives technology, particularly tobacco additives, and one set for their preparation and application for the production of W cigarettes, in particular tobacco additives, and one provided by spraying a solution of cut tobacco.

背景技术 Background technique

[0002] 卷烟燃烧锥溫度是影响主、测流烟气中的化学成分及含量进而影响卷烟燃烧品质的最基本特性参数之一。 [0002] Bevel cigarette combustion temperature is the main chemical composition and content of the flue gas flow measurement thereby affecting the quality of one of the fundamental parameters of the burning cigarette. 它直接影响着燃烧锥之后烟草成分的热解合成反应,影响了卷烟中各类挥发、半挥发成分向烟气中的输送量,也与烟气中有害成分的多少有很大的关联。 It directly affects the composition of the solution after the heat of tobacco combustion cone synthesis reaction, affecting all types of cigarettes in the volatile, semi-volatile components in the feeding amount of flue gas, but also with how much smoke harmful ingredients have great relevance. 随着卷烟燃烧溫度的升高,CO的释放量几乎呈线性增加;在"卷烟烟丝热裂解产物香味成分分析"各种报道和论文中,W及科学实验证实,随着燃烧锥溫度的降低,香味物质释放量的降低幅度很小。 As the firing temperature rises cigarette, CO release amount increases almost linearly; the "cut tobacco pyrolysis products flavor component analysis" various reports and papers, W, and scientific experiments confirmed that with reduced temperature combustion cone, reducing the amplitude of the aroma emission amount is small. 综上所述,降低卷烟燃烧溫度,可W减少卷烟烟气中有害成分的释放量,同时香味物质释放量几乎不受影响。 In summary, reducing the combustion temperature of tobacco, W can reduce the emission of harmful components of cigarette smoke, while the aroma release is hardly affected.

[0003] 目前,在如何降低卷烟燃烧锥溫度上依然是个大难题,在卷烟燃烧使用时,由于正常燃烧的溫度会产生较多的有害物质,对人体危害较大;由于燃烧溫度跟卷烟有害物质的释放成正比,同时,降低溫度对卷烟的抽吸品质影响不大,故如何降低卷烟燃烧的溫度,对环境的保护和抽烟者的健康非常有利。 [0003] At present, how to reduce the temperature of the cigarette burning cone is still a major problem when burning cigarette use, due to the normal combustion temperatures will produce more harmful substances, harmful to the human body; the combustion temperature with cigarette harmful substances release proportional, while not reducing the quality of the suction effect of temperature on cigarettes, so how to reduce cigarette combustion temperature, very beneficial to health protection and smoker's environment.

[0004] 现在,卷烟燃烧测溫技术也得到了飞速发展,利用RM/PLUS单孔道吸烟机配合高分辨的、快速纪录的红外热像仪有效测量出卷烟的燃烧锥溫度。 [0004] Now, a cigarette combustion temperature has been the rapid development of technology, the use of RM / PLUS hole channel smoking machine with high-resolution, fast infrared camera records the measured effective temperature combustion cone cigarette. 吴菊民在2004研制了一种超细测溫热电偶,通过接触法测量烟丝燃烧锥溫度。 Wuju Min in 2004 developed a superfine thermocouple, measuring the temperature by contact cone tobacco combustion method. 由此可见,通过精准的测溫手段,探寻有效降低卷烟燃烧锥溫度的烟丝添加剂,进而减少卷烟燃烧产物中有害成分的释放量,最终实现卷烟的减害降焦,可W解决卷烟燃烧锥溫度的难题。 Thus, through accurate temperature measurement means, seek to reduce the cigarette burning cone temperature effective tobacco additives, thereby reducing emissions of harmful products of combustion of cigarette components, and ultimately harm reduction tar cigarette, the cigarette can burn cone temperature solution W problem.

发明内容阳0化]针对现有技术存在的不足之处,本发明的目的在于提供一种烟丝添加剂的其制备方法W及用于生产卷烟的应用,该烟丝添加剂绿色无害,能够有效降低卷烟燃烧锥溫度,并且制备方法简便易于控制。 Summary of the male 0] for the shortcomings of the prior art, an object of the present invention is to provide a method of preparing tobacco additives and W for the manufacture of cigarettes, the tobacco green harmless additive, can effectively reduce cigarette burning cone temperature, and easy to control and easy preparation.

[0006] 本发明的目的通过下述技术方案实现: [0006] The object of the present invention are achieved by the following technical scheme:

[0007] 一种烟丝添加剂,该烟丝添加剂是由石墨締氧化物通过超声波分散于水中并得到石墨締氧化物浓度为0.Iwt%~0. 3wt%的均相溶液。 [0007] A tobacco additives, the tobacco additive is dispersed in water and ultrasonic waves to obtain a graphite oxide concentration of associative 0.Iwt% ~ 0. 3wt% of the homogeneous solution of graphite oxide by association.

[0008] 一种烟丝添加剂的制备方法,该制备方法采用=步氧化反应制造出石墨締氧化物,然后将石墨締氧化物通过超声波分散于水中形成石墨締氧化物质量数为0.Iwt%~ 0. 3wt%的均相溶液;其制备方法包括如下步骤: [0008] A method of preparing tobacco additives, the production method using an oxidation reaction step for producing a = association graphite oxide, graphite and graphite oxide forms association association oxide mass number 0.Iwt% dispersed in water by ultrasonic ~ 0. 3wt% of a homogeneous solution; the process comprising the steps of:

[0009] 曰、低溫氧化反应:向6~12重量份的石墨粉中加入255~325重量份的浓H2SO4 和2. 5~6. 5重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入22. 5~37. 5重量份的KMn〇4,在低于20°C溫度条件下反应得到低溫氧化溶液; [0009] Said low-temperature oxidation reaction is: 6 to 12 parts by weight of the graphite powder was added 255 to 325 parts by weight of concentrated H2SO4 and 2.5 ~ 65 parts by weight of NaN〇3, then stirred in an ice-water bath embrace. to give a uniform mixed solution was added 22.5 parts by weight of ~ 375 KMn〇4 to the mixed solution, the reaction solution was low-temperature oxidation at a temperature below 20 ° C.;

[0010] b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加8~28重量份的去离子水继续揽拌12~20分钟得到中溫氧化反应溶液; [0010] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to embrace stirred for 35 minutes then add 8 to 28 parts by weight of deionized water continues to embrace mix 12 to 20 minutes the reaction solution obtained in the oxidation temperature;

[0011] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48~70°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; [0011] C, high temperature oxidation reaction: the temperature of step b was placed under the oxidation reaction temperature condition of 48 ~ 70 ° C was added of & until the reaction solution to remove excess KMn〇4;

[0012]t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400rpm条件下离屯、处理7~15分钟,得到粉末状石墨締氧化物; [0012] t from Tun process: The reaction solution obtained from Step C Tun Tun off speed, is 7000 ~ 7400rpm machine conditions, for 7 to 15 minutes to obtain a powdery graphite oxide associated;

[0013] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中。 [0013] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water.

[0014] 本烟丝添加剂制备方法进一步优选的技术方案如下:其制备方法包括如下步骤: [0014] The present method of preparing tobacco additives further preferred technical solution is as follows: The preparation method comprises the following steps:

[0015] 曰、低溫氧化反应:向8~10重量份的石墨粉中加入260~320重量份的浓H2SO4 和3~6重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入24~ 36重量份的KMn〇4,在低于20°C溫度条件下反应得到低溫氧化溶液; [0015] Said low-temperature oxidation reaction is: - 8 to 10 parts by weight of a graphite powder of 260 to 320 parts by weight of concentrated H2SO4 and 3 to 6 parts by weight of NaN〇3 added, and then stirred in an ice-water bath embrace uniformly mixed solution , added to the mixed solution of 24 to 36 parts by weight KMn〇4, at a temperature below 20 ° C reaction temperature oxidation solution;

[0016] b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加10~25重量份的去离子水继续揽拌13~17分钟得到中溫氧化反应溶液; [0016] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to embrace stirred for 35 minutes and then add 10 to 25 parts by weight of deionized water continues to embrace mix 13 to 17 minutes to obtain an oxidation reaction temperature in the solution;

[0017] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度50~60°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; [0017] C, the high temperature oxidation: The oxidation temperature of step b was placed in the reaction temperature condition of 50 ~ 60 ° C was added of & until the reaction solution to remove excess KMn〇4;

[0018] t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400巧m条件下离屯、处理8~12分钟,得到粉末状石墨締氧化物; [0018] t from Tun process: the reaction solution obtained in the step C from the rotational speed Tun, Tun machine is from 7000 - 7400 m clever conditions, for 8 to 12 minutes to obtain a powdery graphite oxide associated;

[0019] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中。 [0019] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water.

[0020] 本发明在完成步骤e之后还进一步优选的技术方案是:所述步骤e之后还进行步骤f,步骤f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0020] In the present invention, after completion of step e is further preferred technical solution: the further step performed after step f e, Step f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additive.

[0021] 本发明中步骤a进一步优选的技术方案是:所述步骤a中石墨粉的粒度控制在400目~800目。 [0021] In the present invention, a step is further preferred technical solution: the step size control of a graphite powder of 400 mesh to 800 mesh.

[0022] 本发明中步骤d进一步优选的技术方案是:所述步骤d离屯、处理后的粉末状石墨締氧化物经过溫水反复漂洗,直到PH值为6.8~7.2,再进行干燥处理。 [0022] In the present invention, step d is further preferred technical solution: the step d from the village, powdered graphite oxide after the associated processing pass rinsed repeatedly with warm water until the PH value of 6.8 to 7.2, and then dried.

[0023] 本发明中步骤e进一步优选的技术方案是:所述步骤e的液态烟丝添加剂中石墨締氧化物在水溶液中的质量数为0.Iwt%~0. 3wt%。 [0023] In the present invention, the step e is further preferred technical solution: the number of the liquid mass of step e tobacco association graphite oxide additives in the aqueous solution is 0.Iwt% ~ 0 3wt%..

[0024] 一种烟丝添加剂在生产卷烟上的应用,用高压喷雾器将烟丝添加剂均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度22±2°C和相对湿度为60±5%RH的平衡箱中平衡65~ 79小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品。 [0024] Application of a tobacco additives in the production of cigarettes, cut tobacco with a high pressure spray additive is uniformly sprayed on the surface of the cigarette tobacco, and then tobacco subjected to a temperature 22 ± 2 ° C and a relative humidity of 60 ± 5% RH equilibrium equilibrate 65 to 79 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine.

[00巧]为了其应用效果更佳,所述烟丝添加剂均相溶液与烟丝的重量份数比为0.OOl~ 0. 003。 [Qiao 00] In order to better effect the application, parts by weight of a homogeneous solution with the tobacco cut filler additive ratio 0.OOl ~ 0. 003.

[0026] 本发明较现有技术相比,具有W下优点及有益效果: [0026] The present invention compared with the prior art, has the following advantages and beneficial effects W:

[0027] (1)本发明的烟丝控溫添加剂属于绿色无害添加剂,其制备过程简便、易于控制, 可根据需要进行批量生产。 [0027] (1) Temperature tobacco additives of the present invention are green harmless additives, which preparation process is simple, easy to control, it may be required for mass production.

[0028] (2)本发明烟丝控溫添加剂的添加方式简便,无须改变现有卷烟生产工艺,原料成本低廉,具有较好的工业应用价值。 [0028] (2) the tobacco temperature was added additives embodiment of the present invention is simple, without changing the conventional cigarette manufacturing process, low raw material cost, has good industrial application value.

[0029] (3)经过多次试验结果表明,将本发明的烟丝添加剂加入现有多款成品烟烟丝中,均有较好的降溫效果,其平均降低溫度为30~45°C,最大幅度降低卷烟抽吸最高溫度79°C;有效地降低了卷烟燃烧的有害物质释放,并且卷烟在燃烧抽吸质量上几乎无变化。 [0029] (3) After several tests results show that the additive of the invention added to the tobacco prior in tobacco variety, have good cooling effect, reducing the average temperature is 30 ~ 45 ° C, the most significant reducing the maximum temperature of the suction cigarette 79 ° C; effectively reduces the release of harmful substances in the cigarette burning, and little change in cigarette smoking quality of combustion.

附图说明 BRIEF DESCRIPTION

[0030] 图1为扫描电镜表征GO包覆烟丝表面后的效果; [0030] FIG. 1 is a scanning electron microscope to characterize the effect of tobacco post-GO-coated surface;

[0031] 图2-1为空白卷烟燃烧锥抽吸最高溫度瞬时溫度分布直观图; [0031] FIG. 2-1 is a suction cone blank cigarette combustion temperature maximum instantaneous temperature profile pictorial diagram;

[0032] 图2-2为试样烟a燃烧锥抽吸最高溫度瞬时溫度分布直观图; [0032] FIG. 2-2 is a sample smoke suction cone combustion temperature maximum instantaneous temperature profile pictorial diagram;

[0033] 图2-3为试样烟b燃烧锥抽吸最高溫度瞬时溫度分布直观图; [0033] FIG. 2-3 is a sample b smoke combustion temperature maximum instantaneous temperature of the suction cone profile pictorial diagram;

[0034] 图2-4为试样烟C燃烧锥抽吸最高溫度瞬时溫度分布直观图; [0034] FIG. 2-4 C a sample cigarette combustion maximum temperature of the suction cone instantaneous temperature profile pictorial diagram;

[0035] 图2-5为试样烟d燃烧锥抽吸最高溫度瞬时溫度分布直观图; [0035] FIG. 2-5 is a sample cigarette combustion d suction cone maximum instantaneous temperature profile intuitive FIG temperature;

[0036] 图2-6为试样烟e燃烧锥抽吸最高溫度瞬时溫度分布直观图; [0036] FIG. 2-6 is a sample e smoke suction cone maximum combustion temperature instantaneous temperature profile pictorial diagram;

[0037] 图2-7为试样烟f燃烧锥抽吸最高溫度瞬时溫度分布直观图。 [0037] FIG. 2-7 is a sample smoke suction cone f combustion temperature maximum instantaneous temperature profile intuitive FIG.

具体实施方式 detailed description

[0038] 下面结合实施例对本发明作进一步地详细说明: [0038] The following embodiments in conjunction with embodiments of the present invention will be described in further detail:

[0039] 实施例 [0039] Example

[0040] 一种烟丝添加剂,该烟丝添加剂是由石墨締氧化物通过超声波分散于水中并得到石墨締氧化物浓度为0.Iwt%~0. 3wt%的均相溶液。 [0040] A tobacco additives, the tobacco additive is dispersed in water and ultrasonic waves to obtain a graphite oxide concentration of associative 0.Iwt% ~ 0. 3wt% of the homogeneous solution of graphite oxide by association.

[0041] 如图1、图2-1~图2-7所示,一种烟丝添加剂的制备方法,该制备方法采用=步氧化反应法制造出石墨締氧化物,然后将石墨締氧化物通过超声波分散于水中形成石墨締氧化物质量数为0.Iwt%~0. 3wt%的均相溶液;其制备方法包括如下步骤: [0041] 1, 2-1 to 2-7, the method for producing a tobacco additives, the production method using an oxidation reaction step = SYSTEM create associative graphite oxide, and graphite oxide by association ultrasonic dispersion association graphite oxide in water to form a mass number 0.Iwt% ~ 0 3wt% of a homogeneous solution; the process comprising the steps of:

[0042] 曰、低溫氧化反应:向6~12重量份的石墨粉中加入255~325重量份的浓H2SO4 和2. 5~6. 5重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入22. 5~37. 5重量份的KMn〇4,在低于20°C溫度条件下反应得到低溫氧化溶液; [0042] Said low-temperature oxidation reaction is: 6 to 12 parts by weight of the graphite powder was added 255 to 325 parts by weight of concentrated H2SO4 and 2.5 ~ 65 parts by weight of NaN〇3, then stirred in an ice-water bath embrace. to give a uniform mixed solution was added 22.5 parts by weight of ~ 375 KMn〇4 to the mixed solution, the reaction solution was low-temperature oxidation at a temperature below 20 ° C.;

[0043] b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加8~28重量份的去离子水继续揽拌12~20分钟得到中溫氧化反应溶液; [0043] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to embrace stirred for 35 minutes then add 8 to 28 parts by weight of deionized water continues to embrace mix 12 to 20 minutes the reaction solution obtained in the oxidation temperature;

[0044] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48~70°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; [0044] C, high temperature oxidation reaction: the temperature of step b was placed under the oxidation reaction temperature condition of 48 ~ 70 ° C was added of & until the reaction solution to remove excess KMn〇4;

[0045]t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400rpm条件下离屯、处理7~15分钟,得到粉末状石墨締氧化物; [0045] t from Tun process: The reaction solution obtained from Step C Tun Tun off speed, is 7000 ~ 7400rpm machine conditions, for 7 to 15 minutes to obtain a powdery graphite oxide associated;

[0046]e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中。 [0046] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water.

[0047] 根据上述制备方法步骤,本实施例进一步优选的制备方法包括如下步骤: [0047] The above preparation method step, preparing a further preferred embodiment of the present embodiment comprises the steps of:

[0048] 曰、低溫氧化反应:向8~10重量份的石墨粉中加入260~320重量份的浓H2SO4 和3~6重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入24~ 36重量份的KMn〇4,在低于20°C溫度条件下反应得到低溫氧化溶液; [0048] Said low-temperature oxidation reaction is: - 8 to 10 parts by weight of a graphite powder of 260 to 320 parts by weight of concentrated H2SO4 and 3 to 6 parts by weight of NaN〇3 added, and then stirred in an ice-water bath embrace uniformly mixed solution , added to the mixed solution of 24 to 36 parts by weight KMn〇4, at a temperature below 20 ° C reaction temperature oxidation solution;

[0049]b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加10~25重量份的去离子水继续揽拌13~17分钟得到中溫氧化反应溶液; [0049] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to embrace stirred for 35 minutes and then add 10 to 25 parts by weight of deionized water continues to embrace mix 13 to 17 minutes to obtain an oxidation reaction temperature in the solution;

[0050] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度50~60°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; [0050] C, the high temperature oxidation: The oxidation temperature of step b was placed in the reaction temperature condition of 50 ~ 60 ° C was added of & until the reaction solution to remove excess KMn〇4;

[0051] t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400巧m条件下离屯、处理8~12分钟,得到粉末状石墨締氧化物; [0051] t from Tun process: the reaction solution obtained in the step C from the rotational speed Tun, Tun machine is from 7000 - 7400 m clever conditions, for 8 to 12 minutes to obtain a powdery graphite oxide associated;

[0052] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中。 [0052] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water.

[0053] 本发明在完成了步骤ae之后,还可W优选进行步骤f,步骤f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0053] In the present invention, after completion of step AE, W is preferably also step F, step f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[0054] 根据本发明优选的一个步骤a实施例,步骤a中石墨粉的粒度控制在400目~800 目。 [0054] According to a preferred embodiment of the present invention, an embodiment of a step, a step to control the particle size of graphite powder of 400 mesh to 800 mesh. 阳化5] 根据本发明优选的一个步骤d实施例,步骤d离屯、处理后的粉末状石墨締氧化物经过溫水反复漂洗,直到PH值为6.8~7.2,再进行干燥处理。 Yang 5] According to the present invention a preferred embodiment, step d, from step d Tun, powdered graphite oxide after the associated processing pass rinsed repeatedly with warm water until the PH value of 6.8 to 7.2, and then dried.

[0056] 根据本发明优选的一个步骤e实施例,步骤e的液态烟丝添加剂中石墨締氧化物在水溶液中的质量数为0.Iwt%~0. 3wt%。 [0056] e according to a preferred embodiment of the present invention, a step number of step e liquid tobacco mass of graphite oxide additives association in an aqueous solution of 0.Iwt% ~ 0. 3wt%.

[0057] 一种烟丝添加剂在生产卷烟上的应用,用高压喷雾器将烟丝添加剂均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度22 + 2°C和相对湿度为60 + 5%RH的平衡箱中平衡65~ 79小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品。 [0057] Application of a tobacco additives in the production of cigarettes, cut tobacco with a high pressure spray additive is uniformly sprayed on the surface of the cigarette tobacco, and then tobacco subjected to a temperature 22 + 2 ° C and a relative equilibrium humidity of 60 + 5% RH equilibrate 65 to 79 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine.

[0058] 为了使得烟丝添加剂在卷烟上应用得更佳,其烟丝添加剂均相溶液与烟丝的重量份数比为0.001~0.003。 [0058] In order to make the application on cigarette tobacco additives have better, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio is from 0.001 to 0.003.

[0059] 本发明的烟丝添加剂在生产卷烟上的应用具体实施例如下: W60] 实施例1 [0059] Application specific embodiment of the present invention is cut tobacco additives in the production of cigarettes for example: W60] Example 1

[0061] 首先制备烟丝添加剂,其制备方法如下: [0061] tobacco additives is first prepared, which was prepared as follows:

[0062] 曰、低溫氧化反应:向6重量份的石墨粉中加入255重量份的浓H2SO4和2. 5重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入22. 5重量份的KMnCV 在低于20°C溫度条件下反应得到低溫氧化溶液; [0062] Said low-temperature oxidation: 6 parts by weight of the graphite powder in 255 parts by weight of concentrated H2SO4 and 2.5 parts by weight of NaN〇3 added, and then stirred in an ice bath embrace a uniform mixed solution, the mixed solution was added 22.5 parts by weight of a low-temperature oxidation reaction KMnCV solution at a temperature below 20 ° C;

[0063]b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加8~28重量份的去离子水继续揽拌12~20分钟得到中溫氧化反应溶液; [0063] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to embrace stirred for 35 minutes then add 8 to 28 parts by weight of deionized water continues to embrace mix 12 to 20 minutes the reaction solution obtained in the oxidation temperature;

[0064] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48~70°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; 阳0化]t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400rpm条件下离屯、处理7~15分钟,得到粉末状石墨締氧化物; [0064] C, high temperature oxidation reaction: the temperature of step b was placed under the oxidation reaction temperature condition of 48 ~ 70 ° C was added of & until the reaction solution to remove excess KMn〇4; 0 of the male] t from Tun, the process: the reaction solution obtained from step C Tun Tun off speed, is 7000 ~ 7400rpm machine conditions, for 7 to 15 minutes to obtain a powdery graphite oxide associated;

[0066] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0.06~ 0. 08W/cm3的超声波分散于水中; [0066] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency is associated oxide 0.06 ~ 0. 08W / cm3 ultrasonic dispersion in water;

[0067]f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0067] f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[0068]如图2-2所示,通过上述步骤得到试样烟a,然后在生产卷烟时,通过高压喷雾器将试样烟a均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度22 ± 2°C和相对湿度为60 ± 5 % RH的平衡箱中平衡65~79小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品,其烟丝添加剂均相溶液与烟丝的重量份数比为0.OOl~0. 003。 [0068] shown in Figure 2-2, the sample obtained by the above steps a cigarette, then in the production of cigarette smoke through a high pressure spray sample was sprayed evenly on the surface of cigarette tobacco, and then tobacco subjected to a temperature 22 ± 2 ° C and a relative humidity of 60 ± 5% RH equilibrium balance tank 65 to 79 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio 0.OOl ~ 0. 003. W例实施例2 阳070] 首先制备烟丝添加剂,其制备方法如下: Example 2 W male 070] tobacco additives is first prepared, which was prepared as follows:

[0071] 曰、低溫氧化反应:向8重量份的石墨粉中加入260重量份的浓H2SO4和3重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入24重量份的KMnCV在低于20°C溫度条件下反应得到低溫氧化溶液; [0071] Said low-temperature oxidation reaction: 8 parts by weight of the graphite powder in 260 parts by weight of concentrated H2SO4 NaN〇3 and 3 parts by weight was added, and then stirred in an ice-water bath embrace a uniform mixed solution obtained, was added to the mixed solution 24 parts by weight of a low-temperature oxidation reaction KMnCV solution below 20 ° C temperature conditions;

[0072]b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加10重量份的去离子水继续揽拌12~20分钟得到中溫氧化反应溶液; [0072] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to 35 minutes embrace mixed, further added 10 parts by weight of deionized water were mixed with 12 to continue to embrace 20 minutes the reaction solution obtained in the oxidation temperature;

[0073] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48~70°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; [0073] C, high temperature oxidation reaction: the temperature of step b was placed under the oxidation reaction temperature condition of 48 ~ 70 ° C was added of & until the reaction solution to remove excess KMn〇4;

[0074]t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400rpm条件下离屯、处理7~15分钟,得到粉末状石墨締氧化物; [0074] t from Tun process: The reaction solution obtained from Step C Tun Tun off speed, is 7000 ~ 7400rpm machine conditions, for 7 to 15 minutes to obtain a powdery graphite oxide associated;

[00巧]e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中; [00 Qiao] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water;

[0076]f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0076] f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[0077] 如图2-3所示,通过上述步骤得到试样烟b,然后在生产卷烟时,通过高压喷雾器将试样烟b均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度22 ± 2°C和相对湿度为60 ± 5 % RH的平衡箱中平衡65~79小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品,其烟丝添加剂均相溶液与烟丝的重量份数比为0.OOl~0. 003。 [0077] As shown in FIG 2-3, a sample obtained by the above step b smoke, and in the production of cigarettes, by the high pressure spray sample was sprayed evenly tobacco smoke b cigarette surface, then placed in a temperature of 22 ± tobacco 2 ° C and a relative humidity of 60 ± 5% RH equilibrium balance tank 65 to 79 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio 0.OOl ~ 0. 003. 阳〇7引实施例3 阳079] 首先制备烟丝添加剂,其制备方法如下: Example 3 Primer male male 〇7 079] tobacco additives is first prepared, which was prepared as follows:

[0080] 曰、低溫氧化反应:向9重量份的石墨粉中加入290重量份的浓H2SO4和4. 5重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入24重量份的KMnCV在低于20°C溫度条件下反应得到低溫氧化溶液; [0080] Said low-temperature oxidation: 9 parts by weight of the graphite powder in 290 parts by weight of concentrated H2SO4 and 4.5 parts by weight of NaN〇3 added, and then stirred in an ice bath embrace a uniform mixed solution, the mixed solution was added 24 parts by weight of a low-temperature oxidation reaction KMnCV solution at a temperature below 20 ° C;

[0081] b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度45°C的恒溫水浴中揽拌35 分钟,再添加17. 5重量份的去离子水继续揽拌20分钟得到中溫氧化反应溶液; [0081] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 45 ° C in embrace stirred for 35 minutes and then was added 17.5 parts by weight of deionized water, stirred for 20 minutes to continue to embrace obtained in The reaction temperature of the oxidation solution;

[0082]C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48 °C条件下加入&〇2,直到除去反应溶液中多余的KMn〇4为止; [0082] C, the high temperature oxidation: The oxidation temperature of step b & 〇2 reaction solution was added at a temperature of 48 ° C conditions, the reaction solution until excess KMn〇4 removed;

[0083]t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7400rpm条件下离屯、处理7分钟,得到粉末状石墨締氧化物; [0083] t from Tun process: The reaction solution obtained from Step C Tun Tun off rotational speed, 7400rpm conditions for the machine, for 7 minutes to obtain a powdery graphite oxide associated;

[0084] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06W/ cm3的超声波分散于水中; [0084] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06W / cm3 ultrasonic dispersion in water;

[00化]f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [Of 00] f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[0086] 如图2-4所示,通过上述步骤得到试样烟c,然后在生产卷烟时,通过高压喷雾器将试样烟C均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度22°C和相对湿度为60%RH的平衡箱中平衡65小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品,其烟丝添加剂均相溶液与烟丝的重量份数比为0.001。 [0086] 2-4, the sample obtained by the above step c smoke, and in the production of cigarettes, by the high pressure spray sample was sprayed evenly tobacco smoke C surface of the cigarette, the tobacco and then placed in a temperature of 22 ° C and a relative humidity of 60% RH equilibrium balance tank for 65 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio is 0.001.

[0087] 实施例4 阳08引首先制备烟丝添加剂,其制备方法如下: Primer tobacco additives is first prepared in Example 4 08 male [0087] embodiment, was prepared as follows:

[0089] 曰、低溫氧化反应:向12重量份的石墨粉中加入290重量份的浓H2SO4和4. 5重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入30重量份的KMnCV 在低于20°C溫度条件下反应得到低溫氧化溶液; [0089] Said low-temperature oxidation reaction: To 12 parts by weight of graphite powder in 290 parts by weight of concentrated H2SO4 and 4.5 parts by weight of NaN〇3 added, and then stirred in an ice bath embrace a uniform mixed solution, the mixed solution was added 30 parts by weight of a low-temperature oxidation reaction KMnCV solution at a temperature below 20 ° C;

[0090] b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35°C的恒溫水浴中揽拌35 分钟,再添加10重量份的去离子水继续揽拌20分钟得到中溫氧化反应溶液; [0090] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ° C in embrace stirred for 35 minutes and then add 10 parts by weight of deionized water, stirred for 20 minutes to continue to embrace obtained in isothermal oxidation The reaction solution;

[0091]C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48°C条件下加入&〇2,直到除去反应溶液中多余的KMn〇4为止; [0091] C, the high temperature oxidation: The oxidation temperature of step b & 〇2 reaction solution was added at a temperature of 48 ° C conditions, the reaction solution until excess KMn〇4 removed;

[0092]t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7400rpm条件下离屯、处理15分钟,得到粉末状石墨締氧化物; [0092] t from Tun process: The reaction solution obtained from Step C Tun Tun off rotational speed, 7400rpm conditions for the machine, for 15 minutes to obtain a powdery graphite oxide associated;

[0093] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 08W/ cm3的超声波分散于水中; [0093] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 08W / cm3 ultrasonic dispersion in water;

[0094]f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0094] f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[00巧]如图2-5所示,通过上述步骤得到试样烟d,然后在生产卷烟时,通过高压喷雾器将试样烟d均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度20°C和相对湿度为55%RH的平衡箱中平衡65小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品,其烟丝添加剂均相溶液与烟丝的重量份数比为0. 003。 [Qiao 00] 2-5, a sample obtained by the above step d smoke, and in the production of cigarettes, by the high pressure spray sample was sprayed evenly tobacco smoke d of the surface of the cigarette, the tobacco and then placed in a temperature of 20 ° C and a relative humidity of 55% RH equilibrium balance tank for 65 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio 0.003 .

[0096] 实施例5 [0096] Example 5

[0097] 首先制备烟丝添加剂,其制备方法如下: [0097] tobacco additives is first prepared, which was prepared as follows:

[0098] 曰、低溫氧化反应:向28重量份的石墨粉中加入325重量份的浓H2SO4和6. 5重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入37. 5重量份的KMnCV 在低于20°C溫度条件下反应得到低溫氧化溶液; [0098] Said low-temperature oxidation reaction: To 28 parts by weight of graphite powder in 325 parts by weight of concentrated H2SO4 and 6.5 parts by weight of NaN〇3 added, and then stirred in an ice bath embrace a uniform mixed solution, the mixed solution was added 37.5 parts by weight of a low-temperature oxidation reaction KMnCV solution at a temperature below 20 ° C;

[0099]b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度45°C的恒溫水浴中揽拌25 分钟,再添加25重量份的去离子水继续揽拌20分钟得到中溫氧化反应溶液; [0099] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 45 ° C in embrace stirred 25 minutes, then adding 25 parts by weight of deionized water, stirred for 20 minutes to continue to embrace obtained in isothermal oxidation The reaction solution;

[0100] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度70°C条件下加入&〇2,直到除去反应溶液中多余的KMn〇4为止; 阳101] t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7200rpm条件下离屯、处理8分钟,得到粉末状石墨締氧化物; [0100] C, the high temperature oxidation: The oxidation temperature of step b & 〇2 reaction solution was added at a temperature of 70 ° C conditions, the reaction solution until excess KMn〇4 removed; male 101] t from the village, processing: the reaction solution obtained from step C Tun Tun off rotational speed, 7200rpm conditions for the machine, for 8 minutes to obtain a powdery graphite oxide associated;

[0102] e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 07W/ cm3的超声波分散于水中; [0102] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 07W / cm3 ultrasonic dispersion in water;

[0103]f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0103] f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[0104] 如图2-6所示,通过上述步骤得到试样烟e,然后在生产卷烟时,通过高压喷雾器将试样烟e均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度24°C和相对湿度为65%RH的平衡箱中平衡72小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品,其烟丝添加剂均相溶液与烟丝的重量份数比为0.002。 [0104] Figure 2-6, the sample obtained by the above step e smoke, and in the production of cigarettes, by the high pressure spray sample was sprayed evenly tobacco smoke e cigarette surface, then placed in a temperature of 24 ° tobacco C and a relative humidity of 65% RH equilibrium balance tank 72 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio is 0.002. 阳105]实施例6 阳106] 首先制备烟丝添加剂,其制备方法如下: 阳107] a、低溫氧化反应:向18重量份的石墨粉中加入320重量份的浓H2SO4和6重量份的NaN〇3,然后在冰水浴中揽拌均匀得到混合溶液,向混合溶液中加入30重量份的KMnCV在低于20°C溫度条件下反应得到低溫氧化溶液; Male 105] Example 6 male 106] tobacco additives is first prepared, which is prepared as follows: male 107] a, the low-temperature oxidation reaction: 320 parts by weight was added to 18 parts by weight of graphite powder and 6 parts by weight of concentrated H2SO4 in NaN〇 3, and then stirred in an ice bath embrace uniformly mixed solution, 30 parts by weight was added to the mixed solution KMnCV reaction below 20 ° C to give a temperature of the low temperature peroxide solution;

[0108] b、中溫氧化反应:将步骤a的低溫氧化溶液置于溫度35~45°C的恒溫水浴中揽拌25~35分钟,再添加4. 5重量份的去离子水继续揽拌12~20分钟得到中溫氧化反应溶液; [0108] b, the oxidation reaction temperature: the low temperature oxidation step was placed in a constant temperature water bath temperature of 35 ~ 45 ° C in 25 to embrace stirred for 35 minutes and then was added 4.5 parts by weight of deionized water continues to embrace mix 12 to 20 minutes the reaction solution obtained in the oxidation temperature;

[0109] C、高溫氧化反应:将步骤b的中溫氧化反应溶液置于溫度48~70°C条件下加入&化,直到除去反应溶液中多余的KMn〇4为止; [0109] C, high temperature oxidation reaction: the temperature of step b was placed under the oxidation reaction temperature condition of 48 ~ 70 ° C was added of & until the reaction solution to remove excess KMn〇4;

[0110] t离屯、处理:将步骤C得到的反应溶液在离屯、机的转速为7000~7400巧m条件下离屯、处理7~15分钟,得到粉末状石墨締氧化物; 阳111]e、超声波分散:将步骤d得到的粉末状石墨締氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中; [0110] t from Tun process: the reaction solution obtained in the step C from the rotational speed Tun, Tun machine is off, for 7 to 15 minutes at from 7000 to 7400 m clever conditions to obtain a powdery graphite oxide associative; 111 male ] e, ultrasonic dispersion: step d graphite powder obtained by the ultrasonic frequency oxide associative 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water;

[0112] f:将步骤C得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 [0112] f: The Step C freeze liquid tobacco additives, obtained after the drying process fluffy tobacco additives.

[0113] 如图2-7所示,通过上述步骤得到试样烟f,然后在生产卷烟时,通过高压喷雾器将试样烟f均匀喷洒在卷烟的烟丝表面,再将烟丝置于溫度22 ± 2°C和相对湿度为60 ± 5 % RH的平衡箱中平衡65~79小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品,其烟丝添加剂均相溶液与烟丝的重量份数比为0.OOl~0. 003。 [0113] Figure 2-7, the sample obtained by the above step f smoke, and in the production of cigarettes, by the high pressure spray sample was sprayed evenly f smoke cigarette tobacco surface and then placed in a temperature of 22 ± tobacco 2 ° C and a relative humidity of 60 ± 5% RH equilibrium balance tank 65 to 79 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine, parts by weight of an additive which is a homogeneous solution with the tobacco cut filler ratio 0.OOl ~ 0. 003.

[0114] 将上述实施例1-6的试样烟分别进行卷烟燃烧,在卷烟燃烧时测定其卷烟燃烧的溫度值,本发明卷烟燃烧溫度的测定方法包括如下步骤: [0114] The tobacco samples above Examples 1-6 were burning cigarette, the cigarette burning temperature value measured at the time of combustion of the cigarette, the cigarette of the present invention is a combustion method for measuring temperature comprises the steps of:

[0115] 利用M1/PLUS单孔道吸烟机配合高分辨的、快速纪录的红外热像仪测量卷烟阴燃和抽吸时的最高溫度。 [0115] using the M1 / ​​PLUS hole channel smoking machine with high resolution and rapid measurement of the infrared camera records smoldering cigarette and the maximum temperature during aspiration. 调整热像仪和目标物的距离为0.Im,红外探测器的测溫范围选择300~1500°C,调好焦距,红外发射率设置为0. 87,W50化的速度记录卷烟抽吸过程中燃烧锥固相溫度,W抽吸最高溫度与阴燃最高溫度值作为对比参数。 Imager and distance adjustment of the object was 0.Im, selection of the infrared detector temperature range 300 ~ 1500 ° C, adjusted the focus, infrared emissivity is set to 0. 87, W50 of the speed of the recording cigarette suctioning cone solidus temperature combustion, W maximum suction temperature and the maximum temperature smoldering as alignment parameters. 每个品种的卷烟进行十次测量,结果取平均值。 Each species cigarette Ten measurements, and the results averaged.

[0116] 各试样烟支在实验前先进行重量和吸阻的分选,尽量保证其具有可比性。 [0116] Each sample cigarettes prior to the experiment for weight and draw resistance before sorting, which try to ensure comparability. 然后在溫度22±1(TC,湿度60 + 2%RH条件下平衡72h。按照国际标准,吸烟机的单口抽吸容量设置为35^3、抽吸时间为2s、抽吸间隔为60s。并得到表1、表2的空白卷烟与各个试样烟的燃烧溫度测定情况。 72h then equilibrated in TC, humidity of 60 + 2% RH conditions of 22 ± 1 (temperature according to international standards, a single port smoking machine suction capacity is set to 35 ^ 3, the suction time of 2s, 60s interval of suction. And obtained in tables 1 and a combustion temperature of white smoke cigarettes 2 of each sample was measured circumstances.

[0117] 表1烟丝添加剂对卷烟最高抽吸溫度的降溫效果: [0117] Table 1 Additives tobacco cigarette maximum suction temperature cooling effect:

Figure CN104055219BD00101

Figure CN104055219BD00111

[0119] 表2烟丝添加剂对卷烟最高阴燃溫度的降溫效果: [0119] Table 2 Additives tobacco smoldering cigarette maximum temperature of the cooling effect:

Figure CN104055219BD00112

[0121] 表3卷烟纸燃烧调节剂试制卷烟感官质量评吸表(评委人数7人) [0121] Table 3 Quality assessment of cigarette paper cigarette burn adjusting agent trial Sensory suction table (No. 7 judges)

Figure CN104055219BD00113

[0123] 表1得出如下结论:通过添加本制备方法得到的烟丝添加剂生产出的卷烟对卷烟最高抽吸溫度的降溫值范围为30~45°C,表2得出如下结论:通过添加本制备方法得到的烟丝添加剂生产出的卷烟对卷烟最高阴燃溫度的降溫值范围为30~45°C;表3得出如下结论:通过添加本制备方法得到的烟丝添加剂生产出的卷烟在卷烟感官质量上与空白卷烟几乎一致,说明降溫30~45°C范围下卷烟的抽吸质量降低较小,几乎无影响。 [0123] Table 1 the following conclusions: prepared by adding tobacco obtained by the method of the present additive produce the highest cigarette cigarettes pumping cooling temperature range of 30 ~ 45 ° C, Table 2 the following conclusions: By adding this preparation obtained tobacco cigarettes additive produced smoldering cigarette maximum cooling temperature range of 30 ~ 45 ° C; table 3 the following conclusions: obtained by adding tobacco additive of the present production method to produce cigarettes in a cigarette sensory quality almost identical empty cigarette, cigarette smoking quality described under cooling range of 30 ~ 45 ° C decreased less, almost no effect. 阳124]综上对比数据得出,本发明得到的烟丝添加剂的添加方式简便,无须改变现有卷烟生产工艺,原料成本低廉,具有较好的工业应用价值。 Male 124] In summary comparison of data obtained, a simple way to add tobacco additive of the present invention obtained, without changing the conventional cigarette manufacturing process, low raw material cost, has good industrial application value. 多次试验结果表明,将本发明所述的烟丝添加剂加入现有多款成品烟烟丝中,均有较好的降溫效果,最大幅度降低卷烟抽吸最高溫度79°C,平均降溫为30~45°C,有效地降低了卷烟燃烧的有害物质释放,并且卷烟在燃烧抽吸质量上几乎无变化。 Multiple test results show that the tobacco additive is added prior to the present invention in tobacco variety, have good cooling effect, the most significant reduction in the maximum temperature of the suction cigarette 79 ° C, average temperature decreasing from 30 to 45 ° C, effectively reduces the release of harmful substances in the cigarette burning, and little change in cigarette smoking quality of combustion.

[0125] W上所述仅为本发明的较佳实施例而已,并不用W限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。 [0125] W the embodiments of the present invention only the preferred embodiments only, not to limit the invention by W, any modifications within the spirit and principle of the present invention, equivalent substitutions and improvements should be included in the within the scope of the present invention.

Claims (8)

  1. 1. 一种烟丝添加剂的制备方法,其特征在于: 烟丝添加剂是由石墨烯氧化物通过超声波分散于水中并得到石墨烯氧化物浓度为0·lwt%~0· 3wt%的均相溶液其制备方法包括如下步骤: a、 低温氧化反应:向6~12重量份的石墨粉中加入255~325重量份的浓H2S0jP 2. 5~6. 5重量份的NaN03,然后在冰水浴中搅拌均匀得到混合溶液,向混合溶液中加入22. 5~37. 5重量份的ΚΜη04,在低于20°C温度条件下反应得到低温氧化溶液; b、 中温氧化反应:将步骤a的低温氧化溶液置于温度35~45°C的恒温水浴中搅拌25~35分钟,再添加8~28重量份的去离子水继续搅拌12~20分钟得到中温氧化反应溶液; c、 高温氧化反应:将步骤b的中温氧化反应溶液置于温度48~70°C条件下加入H202, 直到除去反应溶液中多余的ΚΜη04为止; d、 离心处理:将步骤c得到的反应溶液在离心机的转速为7000~7400rpm条件下离 1. A method of preparing tobacco additives, characterized in that: the tobacco additive is dispersed in water in an ultrasonic graphene and graphene oxide by an oxide concentration of 0 · lwt% ~ 0 · 3wt% of a homogeneous solution which is prepared the method comprises the steps of: a, low temperature oxidation: to a solution of 6 to 12 parts by weight of graphite powder in concentrated H2S0jP 2. 5 ~ 6 5 ~ 325 parts by weight of 255 parts by weight of NaN03 was added, and then stirred at ice-water bath to obtain a uniform the mixed solution, the mixed solution was added to 22.5 parts by weight of ~ 375 ΚΜη04, low-temperature oxidation reaction solution at a temperature below 20 ° C; B, medium temperature oxidation: the oxidation step was placed in a low-temperature the stirring temperature 35 ~ 45 ° C constant temperature water bath 25 to 35 minutes, then add 8 to 28 parts by weight of deionized water, stirring was continued for 12 to 20 minutes to obtain the temperature of the oxidation reaction solution; C, high temperature oxidation reaction: step b the temperature the reaction temperature of the oxidation added H202 solution was placed under conditions of 48 ~ 70 ° C until the reaction solution to remove excess ΚΜη04; D, centrifugation: the reaction solution obtained in step c the speed of the centrifuge is 7000 ~ 7400rpm conditions from 处理7~15分钟,得到粉末状石墨烯氧化物; e、 超声波分散:将步骤d得到的粉末状石墨烯氧化物通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中。 For 7 to 15 minutes, to obtain graphene oxide powder; E, ultrasonic dispersion: The powder obtained in step d graphene oxide ultrasonic frequency by 0. 06 ~ 0. 08W / cm3 to ultrasonic dispersion in water.
  2. 2. 按照权利要求1所述的烟丝添加剂的制备方法,其特征在于:其制备方法包括如下步骤: a、 低温氧化反应:向8~10重量份的石墨粉中加入260~320重量份的浓H2S0JP3~ 6重量份的NaN03,然后在冰水浴中搅拌均匀得到混合溶液,向混合溶液中加入24~36重量份的ΚΜη04,在低于20°C温度条件下反应得到低温氧化溶液; b、 中温氧化反应:将步骤a的低温氧化溶液置于温度35~45°C的恒温水浴中搅拌25~35分钟,再添加10~25重量份的去离子水继续搅拌13~17分钟得到中温氧化反应溶液; c、 高温氧化反应:将步骤b的中温氧化反应溶液置于温度50~60°C条件下加入H202, 直到除去反应溶液中多余的ΚΜη04为止; d、 离心处理:将步骤c得到的反应溶液在离心机的转速为7000~7400rpm条件下离心处理8~12分钟,得到粉末状石墨烯氧化物; e、 超声波分散:将步骤d得到的粉末状石墨烯氧化物 2. The method of claim 1 prepared according to claim tobacco additives, characterized in that: the method comprising the steps of preparing: a, low-temperature oxidation reaction: 260 was added to 320 parts by weight of a concentrated solution of 8 to 10 parts by weight of graphite powder H2S0JP3 ~ 6 parts by weight of NaN03, then stirred in an ice-water bath uniformly to obtain a mixed solution and adding 24 to 36 parts by weight of ΚΜη04 to the mixed solution, the reaction low temperature peroxide solution at below 20 ° C temperature conditions; B, in the temperature stirred water bath of step a low temperature peroxide solution was placed in a temperature 35 ~ 45 ° C in 25 to 35 minutes, then adding 10 to 25 parts by weight of deionized water, stirring was continued for 13 to 17 minutes to obtain the temperature of the oxidation reaction solution: an oxidation reaction ; c, high temperature oxidation reaction: step b the temperature of the oxidation reaction solution was added H202 at a temperature of 50 ~ 60 ° C conditions, until the reaction solution, excess ΚΜη04 removed; D, centrifugation: the reaction solution obtained in step c the rotational speed of the centrifuge at 7000 to 7400rpm centrifuged for 8 to 12 minutes to obtain a powdery graphene oxide; E, ultrasonic dispersion: the graphene oxide powder obtained in step d 通过超声波频率为0. 06~ 0. 08W/cm3的超声波分散于水中。 Ultrasonic frequency by the ultrasonic 0. 06 ~ 0. 08W / cm3 dispersed in water.
  3. 3. 按照权利要求2所述的烟丝添加剂的制备方法,其特征在于:所述步骤e之后还进行步骤f, 步骤f:将步骤c得到的液态烟丝添加剂经过冷冻、干燥处理后得到蓬松状的烟丝添加剂。 3. The method of claim 2 prepared tobacco additive according to claim, wherein: said further step after step e F, Step f: The freeze-dried to give a fluffy treated liquid obtained in step c tobacco additives tobacco additives.
  4. 4. 按照权利要求2所述的烟丝添加剂的制备方法,其特征在于:所述步骤a中石墨粉的粒度控制在400目~800目。 4. The method of claim 2 prepared according to claim tobacco additives, characterized in that: said step a graphite powder particle size is controlled to 400 mesh to 800 mesh.
  5. 5. 按照权利要求2所述的烟丝添加剂的制备方法,其特征在于:所述步骤d离心处理后的粉末状石墨烯氧化物经过温水反复漂洗,直到PH值为6. 8~7. 2,再进行干燥处理。 5. The method of claim 2 prepared tobacco additive according to claim, wherein: said step d graphene oxide powder after repeated rinsing warm water after centrifugation until PH value of 6.8 - 72, and then dried.
  6. 6. 按照权利要求2所述的烟丝添加剂的制备方法,其特征在于:所述步骤e的液态烟丝添加剂中石墨稀氧化物在水溶液中的质量数为0.lwt%~0. 3wt%。 6. The method of claim 2 prepared tobacco additive according to claim, wherein: said step e of the mass number of the liquid tobacco additives graphene oxide in an aqueous solution of 0.lwt% ~ 0 3wt%..
  7. 7. -种根据权利要求1~6任一项所述制备方法得到的烟丝添加剂在生产卷烟上的应用,其特征在于:用高压喷雾器将烟丝添加剂均匀喷洒在卷烟的烟丝表面,再将烟丝置于温度22±2°C和相对湿度为60±5%RH的平衡箱中平衡65~79小时,最后用工厂卷烟机将平衡后的烟丝卷制成卷烟成品。 7. - The use of any kind of tobacco additive of claim 1 to 6, a preparation obtained by the method in the production of cigarettes, as claimed in claim wherein: a high pressure sprayer tobacco additive is uniformly sprayed on the surface of the cigarette tobacco, and then tobacco counter at a temperature of 22 ± 2 ° C and a relative humidity of 60 ± 5% RH equilibrium balance tank 65 to 79 hours after the final volume with tobacco cigarette factory finished cigarette made balancing machine.
  8. 8. 按照权利要求7所述的烟丝添加剂在生产卷烟上的应用,其特征在于:所述烟丝添加剂均相溶液与烟丝的重量份数比为〇. 001~〇. 003。 Application of the additive in the production of 7 tobacco cigarette according to claim 8, wherein: the tobacco parts by weight of a homogeneous solution with the tobacco additive ratio square square 001 ~ 003...
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CN103537263A (en) * 2013-09-26 2014-01-29 湖南中烟工业有限责任公司 Schiff base surface-grafted graphite oxide compound and preparation method and application thereof

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CN103263077A (en) * 2013-04-24 2013-08-28 湖北中烟工业有限责任公司 Method for preparing cigarette flaky carbonaceous heat source materials by calcium salt
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